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Articles in press have been peer-reviewed and accepted, which are not yet assigned to volumes /issues, but are citable by Digital Object Identifier (DOI).
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Design, synthesis and insecticidal activities of aryloxypyridinyl ethanone oxime ethers
Shijie DU, Dongyan YANG, Chuan WAN, Fenghai ZHAO, Zhaohai QIN
 doi: 10.16801/j.issn.1008-7303.2021.0051
[Abstract](153) [FullText HTML](114) [PDF 527KB](9)
Abstract:
Based on the structure of the plug-in molecule aryloxypyridine methanone, a novel series of aryloxypyridine methanone oxime ethers containing several active units (pyridine, thiazole, diaryl ether, and oxime ether) were synthesized and characterized by 1H NMR, 13C NMR and HRMS. The insecticidal activities were also investigated. The target compounds had moderate to good activity against Aphis gossypii (Glover), while compounds 5a and 6i showed excellent insecticidal activities with the lethal rate of 76.8% and 70.1% at the concentration of 50 μg/mL, respectively. However, the lethal rate of the target compounds was lower than 30% at the concentration of 100 μg/mL, showing poor insecticidal activities against Plutella xylostella. This series of compounds mainly demonstrated the active characteristics of neonicotinoids, and provided a new idea for further study of their structure-activity relationship.
Residual analysis and selective degradation of profenofos enantiomers in citrus
Chao DONG, Jing LI, Qing YANG, Yaohai ZHANG, Qiyang ZHAO, Bining JIAO
 doi: 10.16801/j.issn.1008-7303.2021.0063
[Abstract](38) [FullText HTML](17) [PDF 726KB](5)
Abstract:
An analytical method of the chiral stationary phase/high performance liquid chromatography-tandem mass spectrometry technique coupled with QuEChERS for determination of the enantiomers of profenofos in citrus was developed, and the selective degradation behavior of profenofos enantiomers in citrus was studied through field experiments. The sample preparation involved quick extraction with acetonitrile and cleaning-up with multi-walled carbon nanotube sorbent. The enantiomers of profenofos were separated by a ND (2)-RH chiral column, detected by tandem mass spectrometry in multi-reaction monitoring (MRM) mode, and quantified using matrix-matched calibration curves. The results showed good linear relationships for the analytes in the concentration range of 2.5-250 μg/L with their correlation coefficients (r) >0.999 6. The limits of quantitation (LOQs) were 5 μg/kg. The average recoveries of the two enantiomers of profenofos in citrus ranged from 76% to 83% at three spiked levels(5,100, 500 μg/kg) and the relative standard deviations (RSD) were between 2.6% and 6.0%. Field experiments were conducted to study the differences in the degradation of profenofos enantiomers in citrus. The results of dynamic experiments showed that degradation of the enantiomers of profenofos in citrus conformed to the first-order reaction kinetic equation, and the half-lives of (+)-profenofos and (-)-profenofos were 12.53 d and 14.14 d, respectively. The enantiomer fraction (EF) value of the profenofos enantiomers in the field experiments reached 0.43 after 30 d of application, indicating that there were significant enantio-selectivity in the degradation of profenofos enantiomers in citrus.
Combined toxicity of five pesticides and their binary and ternary mixtures on HepG2 cells
Tiancai WANG, Chen CHEN, Mengmeng MA, Xi YANG, Yun LI, Yongzhong QIAN
 doi: 10.16801/j.issn.1008-7303.2021.0021
[Abstract](175) [FullText HTML](116) [PDF 998KB](2)
Abstract:
To study the combined toxicity of pesticides mixtures in agricultural products, five pesticides with wide application and broad spectrum, including difenoconazole, cypermethrin, dimethomorph, cyhalothrin, acetamiprid, and relevant binary and ternary combinations with high exposure levels in lettuce were selected. Cell Counting Assay Kit-8 method was used to determine the proliferation inhibition toxicity of single pesticide and mixtures on HepG2 hepatocytes. The combined effects were assessed by three prediction models, concentration addition, independent action and combination index, based on the concentration-response curve of individual pesticides. Then the induction effects of two ternary combinations on cell apoptosis were analyzed by High Content Screening. The results showed that the effects of different pesticide combinations on the cell growth inhibitory rate of HepG2 cells were different, all of which had obvious concentration-response relationship. Among them, difenoconazole had a strong inhibition of proliferation toxicity, and the median effective concentration was 24.72 μmol/L. The order of toxicity for the other individual pesticides was ranked as dimethomorph > cyhalothrin > acetamiprid > cypermethrin. The combined toxicity of the pesticide mixtures was determined by the combination index. The results showed that with the increase of pesticide concentrations, the combined effects of all binary combinations changed from antagonism to synergy. While in ternary mixtures, including dimethomorph + difenoconazole + cypermethrin and dimethomorph + cypermethrin + acetamiprid, the combined effects changed from synergy to antagonism when the growth inhibition effect were 60% and 18%, respectively. In addition, the dose reduction index was used to quantify the synergistic effect between pesticide mixtures, indicating that cypermethrin played a greater role in the synergistic effect of the above two ternary combinations. In the measurement of apoptosis toxicity, the apoptotic rate of HepG2 cells significantly increased in the groups treated by individual pesticides in a concentration-dependent manner. The apoptotic rate induced by the ternary combination of dimethomorph + cypermethrin + acetamiprid was significantly increased in concentration between of 20.02-80.10 μmol/L. This work confirmed that the toxicities of proliferation inhibition and apoptosis induction of different pesticides mixtures on HepG2 cells both showed obvious concentration-response relationship, which could provide a scientific basis for toxicity evaluation and risk monitoring of pesticides mixtures. The combination index model as an effective ecotoxicological risk assessment tool can quantitatively describe the interactions of pesticide mixtures under different components and concentrations, which can predict the combined toxicity of pesticide mixtures more accurately compared with the concentration addition model and the independent action model.
Progress in microbial degradation of imidazolinone herbicides
Xin WANG, Jiawen HOU, Wenrui LIU, Jia BAO
 doi: 10.16801/j.issn.1008-7303.2021.0041
[Abstract](402) [FullText HTML](202) [PDF 585KB](5)
Abstract:
Imidazolinone herbicides are widely used in China. Their advantages include wide herbicide spectrum, high activity and strong selectivity, but the pesticide remains in soil for a long time. In this paper, the effects of imidazolinone herbicide residues on succeeding crops were reviewed, and its microbial groups and degradation pathways were investigated. The existing problems and prospects for herbicide remediation were pointed out. It is helpful for the study on the microbial degraders of imidazolinone herbicides.
Efficacy of a novel succinate dehydrogenase inhibitor pydiflumetofen to control rice bakanae disease caused by Fusarium fujikuroi
Yiping HOU, Xiangpu QU, Xiaowei CAI, Luoyu WU, Changjun CHEN, Jianxin WANG, Baohua TIAN, Mingguo ZHOU
 doi: 10.16801/j.issn.1008-7303.2021.0084
[Abstract](13) [FullText HTML](8) [PDF 749KB](6)
Abstract:
Fusarium fujikuroi is the main pathogen causing rice bakanae disease. The fungicide pydiflumetofen is a novel succinate dehydrogenase inhibitor (SDHI). The activity of pydiflumetofen against F. fujikuroi and its efficacy of controlling rice bakanae disease is obscure. In this study, 100 strains of F. fujikuroi were isolated from different regions of Jiangsu and Zhejiang Province in China. The baseline sensitivity of F. fujikuroi to pydiflumetofen was established by mycelial growth assay and spore germination assay respectively, and physiological effect of the fungicide against F. fujikuroi and its control efficacy were investagated. The EC50 (half effective concentration) values of pydiflumetofen on restraining mycelial growth against F. fujikuroi population (n = 100) ranged from 0.0125 μg/mL to 0.1118 μg/mL and the mean value was 0.0503 (± 0.0029) μg/mL. The EC50 values of pydiflumetofen on inhibiting spore germination distributed from 0.0001 μg/mL to 0.0245 μg/mL and the mean value was 0.0038 (± 0.0005) μg/mL. Treated with 0.05 μg/mL (EC50 value) or 1.30 μg/mL (EC90 value) pydiflumetofen, the offshoot of top mycelia of F. fujikuroi increased while sporulation production descreased. The membrane structure and organelles (eg. mitochondria) were damaged and the intracellular plasma leakage increased through imperfect membrane. There was no significant difference in the exopolysaccharides production while peroxidase activity declined after treated with pydiflumetofen. Control efficacy of 10, 15 and 20 g a.i./100 kg seeds of pydiflumetofen against rice bakanae disease by seed dressing is 94.77%, 98.60 % and 100% respectively. Above results indicate that pydiflumetofen has very high activity against F. fujikuroi and is a nice fungicide for controlling rice bakanae disease caused by F. fujikuroi.
Synthesis and herbicidal activity of 4H-pyrazolo[3,4-d][1,2,3]triazine-4-one with bulky substituents
Jian GU, Xiaohan LI, Zhenxue WANG, Yeye CHEN, Xiyue CHEN, Huabin LI
 doi: 10.16801/j.issn.1008-7303.2021.0071
[Abstract](56) [FullText HTML](32) [PDF 538KB](4)
Abstract:
Using 1-(substituted) phenyl-5-amino-1H-pyrazole-4-formate or 1-tert-butyl-5-amino-1H- pyrazole-4-carbonyl chloride and 2-methyl-4-propargyl-6-amino-7-fluoro-2H-benzo[b][1,4]-oxazine- 3(4H)-one as starting material, through different synthetic routes, 22 novel 4H-pyrazolo[3,4-d][1,2,3] triazine-4-ones with bulky substituents were obtained. Their structures were confirmed by HRMS and 1H NMR. Preliminary results showed that all compounds displayed herbicidal activities at a dosage of 375 g /hm2. The inhibition rates of 4h , 4i and 4j against Amaranthus retroflexus were nearly 100%.
Development of prothioconazole + tebuconazole 240 g/kg SC and its control on rice sheath blight and wheat sharp eyespot in the field
Chen CHEN, Kun ZHANG, Tao DING, Jianguo FENG, Jin YANG, Zhen HE, Xijun CHEN
 doi: 10.16801/j.issn.1008-7303.2021.0050
[Abstract](23) [FullText HTML](18) [PDF 570KB](2)
Abstract:
Prothiconazole, a new kind of broad spectrum triazolthione fungicide, was used to develop the suspension concentrate (SC) compounding with tebuconazole. The results of combined virulence determination, adjuvant system screening and physical and chemical properties detection showed that the ratio of prothioconazole to tebuconazole 2 : 1 had high combined virulence against Rhizoctonia solani and Rhizoctonia cerealis, the pathogen of rice sheath blight and wheat sharp eyespot, with the co-toxicity coefficients of 1.91 and 1.92, respectively. The reasonable formula of prothioconazole + tebuconazole 240 g/kg SC was prothioconazole 16.0%, tebuconazole 8.0%, Featdis SCP 4.0%, EFW 3.0%, xanthangum 0.2%, aluminum-magnesium silicate 1.0%, elycol 4.0%, and water up to 100%. After the product was stored at (54 ± 2) ℃ for 14 d, its characters were as follows: suspension rate 95.2%, pH value 6.9, average particle size 0.71 µm, water extraction rate 2.3%, and long-lasting forming ability less than 25 mL. After being stored at (0 ± 2) ℃ for 7 d, its characters were as follows: suspension rate 94.8%, pH value 7.1, average particle size 0.87 µm, long-lasting forming ability less than 25 mL, and viscosity between 200 mPa·s and 600 mPa·s. The field tests indicated that prothioconazole + tebuconazole 240 g/kg SC had good control effect on rice sheath blight and wheat sharp eyespot, and the control effect reached 89.01% and 86.26% at 210 g a.i/hm2 and 150 g a.i/hm2, respectively.
Comparative analysis of the four formulas commonly used for calculating the control efficacy of fungicides on disease in field trials
Xiong LI, Nan ZHANG, Xianbin LI, Tao CANG, Jun YANG, Zhongqiao HUANG, Jianqiang MIAO, Xili LIU
 doi: 10.16801/j.issn.1008-7303.2021.0077
[Abstract](38) [FullText HTML](12) [PDF 622KB](5)
Abstract:
Field efficacy trials are an indispensable part of pesticide registration management, among which, the accuracy and effectiveness of the formulas for calculating control effect of fungicide on plant disease are crucial for the scientific and reasonable evaluation of the field control efficacy of fungicides on plant diseases. At present, the commonly used calculation formulas are different in applicability and calculation errors, and a systematic comparison of commonly used formulas remain unstudied. In this paper four formulas commonly used in field efficacy trials are selected for comparative research. The range of application of the commonly formulae and the stability of the calculation results were accurately evaluated, and the condition indices observed in the disease index after the treatment were corrected. The results show that for given disease indexes of the treated group and the control group, the four formulas have different sensitivity to the initial difference of disease index between the treated group and the control group. When the change of the disease index is extremely small, the calculation results from formula (1), (3) and Yang Xindong's formula (4) do not depend on the disease index of the control group. When the disease index in the treated group is reduced after treatment, the calculation results from formula (1) and (3) are out of the range of corrected efficacy. while Henderson-Tilton formula, formula (2) in the paper, is used to calculate control effect based on the rate of change of the disease index before and after treatment, which can effectively avoid the result deviation or the overflow of the range of corrected efficacy. When the initial disease index is higher in the control group and disease epidemic occurs rapidly, Yang Xindong's formula was recommended for calculatinge the control effect, which can reduce errors caused by the difference in disease index after treatment between treated group and control group. A comprehensive consideration of various influencing factors before and after treatment in field trials indicated that formula (2) is more applicable under the application of fungicides at the early stage of disease development in field.
Research on ecotoxicological effects of succinic dehydrogenase inhibiting fungicides on aquatic organisms
Hong LI, Tongfang JING, Tongbin LI, Beixing LI, Mu WEI
 doi: 10.16801/j.issn.1008-7303.2021.0073
[Abstract](9) [FullText HTML](4) [PDF 578KB](2)
Abstract:
Succinate dehydrogenase inhibitor (SDHIs) fungicides, one of the main players in the current fungicide market, are widely used, which leads to their entry into the aquatic environment and threatens the safety of aquatic organisms. A large number of studies have shown that most of these insecticides have high acute toxicity to aquatic organisms, and some of them even reach the level of severe toxicity. Furthermore, SDHIs have toxic effects on aquatic organisms at a lower concentration, affecting the growth, development and reproduction of aquatic organisms, which can further cause the imbalance of the aquatic ecosystems. The research progress summarizing the pollution influence of SDHIs in the aquatic environment, toxic effects and mechanisms of action to aquatic organisms. Furthermore, the research focus and development direction of the aquatic ecotoxicology of these fungicides in the future are prospected, aiming to provide theoretical basis for reducing the impact of such fungicides on aquatic ecosystems.
Research progress on molecule design and conduction distribution mechanism of guided pesticide
Yongxin XIAO, Junkai LI
 doi: 10.16801/j.issn.1008-7303.2021.0072
[Abstract](17) [FullText HTML](9) [PDF 701KB](4)
Abstract:
Guided pesticide is a kind of that can directionally translocate and accumulate to specified parts in plants. Improving the conductivity of xenobiotics can dramatically enhance systematic distribution of plants and achieve precise control. In this paper, the idea of molecular design of guided pesticide is reviewed, as well as research progress on sugar guided pesticide and amino acid guided pesticide regarding its phloem translocation and biological activities. It is structure-activity relationship (SAR) between pesticide molecule and relevant amino acid transporter that is a research focus for the next few years. A novel guided pesticide taking elicitor as guided group and possessing properties of plant activator is put forward to develop.
High-throughput screening of pesticide residues in Chinese herbal medicines by QuEChERS-GC-MS/MS method
Xuezhe HUANG, Zongyan CUI, Na GE, Yongyan JI, Yanzhong CAO
 doi: 10.16801/j.issn.1008-7303.2021.0083
[Abstract](28) [FullText HTML](18) [PDF 680KB](6)
Abstract:
A database of 460 pesticide residues was established based on gas chromatography tandem mass spectrometry (GC-MS/MS). Being combined with QuEChERS sample preparation technology, it was used for rapid and high-throughput screening of pesticide residues in Chinese herbal medicines. The samples were extracted with 0.1% acetic acid-acetonitrile, cleaned-up by dispersive solid phase extraction with PSA + C18 after salting out with sodium chloride, and then determined by GC-MS/MS. The results showed that the limits of quantification (LOQs) of 421 pesticides in 5 types of Chinese herbal medicine matrices, including rhizome, mosaic, seed, whole grass and bark, were between 0.006 and 221 μg/kg, of which more than 80% of them were less than 50 μg/kg. At the spiking level of 100 μg/kg, the recoveries of more than 72% pesticides were between 60%-120%, and the precision of more than 77% pesticides was within 20%. The method has the advantages of simplicity, rapidity and high throughput, and has achieved the simultaneous detection of more than 400 pesticide residues in one injection. A total of 72 pesticide residues were detected in 215 batches of commercially available samples, among which, the detection rates and the concentrations of chlorpyrifos and cyhalothrin were both high, and their potential risks on quality and safety should be concerned.
Residue mornitoring and crop safety in soil of 5-dialkylamino sulfonylurea compounds
Shaa ZHOU, Jiaxing LI, Xuewen HUA, Yonghong LI, Bin LIU, Anliang CHEN, Jie CHEN, Zhengming LI
 doi: 10.16801/j.issn.1008-7303.2021.0069
[Abstract](13) [FullText HTML](2) [PDF 605KB](0)
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Chlorsulfuron, a representative sulfonylurea herbicide once was widely used for wheat, was banned for its long persistence in soil. Various alternatives have been proposed for chlorsulfuron replacement. Our previous study found that dimethylamino and diethylamino substitutions on the 5th position of sulfonylurea (Compounds Ia and Ib , respectively) could keep high herbicidal activities with accelerating degradation kinetics of sulfonylurea in acidic and alkaline soils. In order to evaluate the field soil degradation, its degradation dynamic was determined in a greenhouse (Cangzhou city, Hebei Province, China, pH 8.46) by Brassica campestris via pot-trials. The growth of B. campestris recovered gradually after Ia and Ib treatments, however, chlorsulfuron showed severe phytotoxicity with 70% of inhibition after 70 days of application (60 g a.i/hm2). As for the application of chlorsulfuron in wheat field and sulfonylureas in cereal field, the wheat and corn safety were tested further. The foliage treatment(15-60 g a.i/hm2) in wheat displayed insignificant inhibition. Meanwhile, the corn safety exhibited beneficial influence that Ia prompted the growth of corn at the concentration of 30-120 g a.i/hm2 under post-emergence. Consequently, the soil degradation dynamic in pot-trials, as well as crop safety, proved the promising application value of Ia and Ib in production.
Screening of pre-emergence herbicides to control a noxious weed Aegilops tauschii in wheat fields
Hengzhi WANG, Kongping ZHAO, Xiaolin ZHANG, Lele ZHANG, Xiuxia DONG, Baolin ZHU, Weitang LIU
 doi: 10.16801/j.issn.1008-7303.2021.0032
[Abstract](391) [FullText HTML](215) [PDF 449KB](9)
Abstract:
Aegilops tauschii, a noxious weed, is widely distributed in winter wheat fields in China. The feasibility of pre-emergence (PRE) chemical control of A. tauschii was studied by the greenhouse and field experiments to find out appropriate PRE herbicides against A. tauschii and provide theoretical foundation for the chemical control of A. tauschii. The results of greenhouse study showed that flufenacet, oxadiazon and isoproturon were effective against A. tauschii, with GR50 values of 37.2, 15.7 and 349.3 g/hm2, respectively, which were all below their field recommended rates. However, their selectivity indexes (Is) were below 2 (0.6-1.1), which suggested poor safety to wheat. The joint effect type was additive when isoproturon was mixed with oxadiazon for the control of A. tauschii. When the mass ratio was 4 : 1 (isoproturon : oxadiazon), the weed control efficacy of the mixtures against A. tauschii was higher than that of isoproturon applied alone, and the safety of the mixtures to tested wheat cultivars was improved when compared with that of oxadiazon or isoproturon used alone with Is of 2.0. The results of the field experiments showed that the PRE application of the mixtures of isoproturon and oxadiazon at 600-900 g/hm2 had 86% efficacy against Bromus japonicus, A. tauschii, Galium aparine and Descurainia sophia at least, increased wheat grain yield by at least 13%, and were safe to the test cultivar of winter wheat.
Chitinase inhibitors and synthesis and agricultural bioactivity of thiazolidinones: a review
Jingyu ZHANG, Qing HAN, Zhiyang JIANG, Huilin LI, Mingfei DENG, Kai ZHU, Mingjun LI, Hongxia DUAN
 doi: 10.16801/j.issn.1008-7303.2021.0049
[Abstract](267) [FullText HTML](191) [PDF 1585KB](11)
Abstract:
Chitinase (EC 3.2.1.14) plays an important role in the chitin metabolism process by degrades chitin into chitooligosaccharides. Chitinase is indispensable for the growth and morphogenesis of agricultural pests and diseases hosts such as insects, fungi, nematodes, etc. Therefore, Chitinase is one of the most promising targets for developing new pesticides with novel molecular mechanism. In recent years, thiazolidinones were reported to possess a variety of agricultural biological activities including chitinase inhibition, so the synthesis methods of thiazolidinones have attracted attention widely. In this review, the chitinases structure represented by those from Ostrinia furnacalis were summaried, as well as the structure of its carbohydrate, peptide, virtual screening, natural-source inhibitors, and their binding mode. The synthesis and agricultural biological activities of three classes of thiazolidinones were reviewed, including thiazolidin-4-ones, 2-thioxothiazolidin-4-ones, and thiazolidin-2,4-diones. Meanwhile, the wide application of thiazolidinones as chitinase inhibitors is prospected. It will provide a guidance for rational designing and discovering novel thiazolidinones as chitinase inhibitors for agricultural pest control based on insect chitinase structure.
Residue and dissipation dynamics of ningnanmycin in ginseng by high performance liquid chromatography-tandem mass spectrometry
Yutong SONG, Yang LU, Qinghang YOU, Xingang HOU, Zongli ZHU, Xiaowei SUN, Nan FANG, Zhiguang HOU, Shuang LIANG, Zhongbin LU
 doi: 10.16801/j.issn.1008-7303.2021.0081
[Abstract](17) [FullText HTML](9) [PDF 464KB](5)
Abstract:
To investigate the dissipation and residues of ningnanmycin in ginseng, field trials of ningnanmycin residues in ginseng and its plants were conducted in Baishan City, Fusong County, Yanji City of Jilin Province, and Huanren County of Liaoning Province in 2019. The samples were extracted by 0.2% formic acid aqueous solution, cleaned up with PLS+PXC solid phase extraction column, separated by XSelect® HSS T3 column, and determined using HPLC-MS/MS. At different spiking levels, the average recoveries of ningnanmycin in fresh ginseng, ginseng plants, and dried ginseng were 90%-99%, 92%-94%, 88%-95%, and the relative standard deviations (RSD) were 4.7%-5.6%, 4.0%-5.6%, and 1.4%-10%, respectively. The limit of quantification (LOQ) of fresh ginseng and ginseng plants were both 0.1 mg/kg, and that of dried ginseng was 0.2 mg/kg. The results of the dissipation dynamic test in Baishan and Huanren showed that the half-lives of ningnanmycin on ginseng plants were 11.77d and 0.76 d. The final residue results in 4 test places showed that the final residues of ningnanmycin on fresh ginseng, ginseng plants, and dried ginseng were <LOQ, <LOQ-0.152 mg/kg, and <LOQ, respectively. The results indicated that the harvested ginseng with the pre-harvest interval of 14 days would be safe for consumption after spraying 8% ningnanmycin AS at the recommended dosage of 675-900 g/hm2 (54-72 g a.i./hm2) 3 times to prevent and treat ginseng disease.
Determination of 13 pyrethroids in water and sediment system by gas chromatography-mass spectrometry
Jian HE, Yezhi DOU, Juying LI, Jia YU, Yueqing ZHANG, Li CAO, Jing XU, Deyang KONG
 doi: 10.16801/j.issn.1008-7303.2017.0000
[Abstract](15) [FullText HTML](6) [PDF 808KB](2)
Abstract:
A residue analytical method was developed for the simultaneous determination of 13 pyrethroid pesticides in water-sediment system. Solid-phase extraction (SPE) and pressurized fluid extraction (PFE) were used as sample preparation method for water and sediment, respectively. Then gas chromatography-mass spectrometry (GC-MS) was used to detect the analytes in selective ion monitor (SIM) mode with internal standard method for quantification. The results showed that the linear relationship for the 13 pyrethroids was good with the correlation coefficient (R2) ≥ 0.995. The recoveries of the pyrethroids were 83%-104% and the relative standard deviation (RSD, n = 6) were 0.73%-6.8% at the spiking levels of 0.50-50 μg/L in water; the recoveries of the pyrethroids were 73%-92% and the relative standard deviation (RSD, n = 6) were 0.63%-5.3% at the spiking levels of 5.0-50 μg/kg in sediment. The detection limits were 1.0-7.0 μg/L, and the quantification limits were 0.50 μg/L and 5.0 μg/kg in water and sediment, respectively. The method is easy to operate with high sensitivity and reliable reproducibility, which is suitable for simultaneous determination of pyrethroid pesticides in water-sediment system.
Residues and dissipation dynamics of butralin in ginseng
Qinghang YOU, Pai PENG, Yutong SONG, Nan FANG, Zongli ZHU, Xingang HOU, Shuang LIANG, Zhongbin LU, Tong QU, Zhiguang HOU
 doi: 10.16801/j.issn.1008-7303.2021.0082
[Abstract](20) [FullText HTML](10) [PDF 608KB](2)
Abstract:
A high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for the determination of the residues of butralin in ginseng was established, and the dissipation dynamics and final residues of butralin in ginseng were investigated. The samples were extracted by acetonitrile, cleaned-up by NH2 solid phase extraction (SPE) cartridges, detected by liquid chromatography-tandem mass spectrometry, and quantified with external standard method. The results showed that in the range of 0.002-0.5 mg/L, there was a good linear relationship between the mass concentration of butralin and the corresponding peak area. The recoveries of butralin were 93%-108% and the relative standard deviations were 0.60%-6.2% at spiking levels of 0.01, 0.05 and 0.5 mg/kg for fresh ginseng and dried ginseng and at spiking levels of 0.01, 0.05, 0.5 and 10 mg/kg for ginseng plant and soil. The half-lives of butralin in ginseng plant and soil were 10.81-18.91 days, and the final residues of butralin in fresh ginseng, dried ginseng, ginseng plant, and ginseng soil were <LOQ-0.010 mg/kg, <LOQ-0.024 mg/kg, 0.011-0.19 mg/kg, and 0.16-0.41 mg/kg, respectively. It is suggested that the maximum residue limit (MRL) of butralin in ginseng could be tentatively set at 0.05 mg/kg, and the harvested ginseng was safe for consumption after the 48% butralin EC was sprayed on the soil surface once at dosage of 3750 g/hm2 (active ingredient of 1800 g/hm2) before the emergence of ginseng seedling.
Effect of Residual Tebuconazole on the Flavor Quality of Different Saccharomyces cerevisiae Simulated Fermentation Process
Shanshan ZHAO, Minmin LI, Ruixing LI, Rui QUAN, Jieyin CHEN, Xiaofeng DAI, Zhiqiang KONG, Jian TIAN
 doi: 10.16801/j.issn.1008-7303.2021.0079
[Abstract](22) [FullText HTML](14) [PDF 602KB](4)
Abstract:
In order to explore the degradation of tebuconazole under the action of different Saccharomyces cerevisiae in wine and the influence of tebuconazole residue on the flavor quality of different Saccharomyces cerevisiae fermentation process, this study added standard solution of tebuconazole to the simulated grape juice medium to 2 mg/L. Then use 12 kinds of wine-making yeast commonly used in production to simulate alcoholic fermentation treatment. Determination of Tebuconazole Residues in Wine by QuEChERS analysis methods. Meanwhile, the electronic nose, electronic tongue and Solid-phase microextraction gas chromatography-mass spectrometry (SPME-GC-MS) were used to analyze the effect of tebuconazole residue on wine flavor quality. The results show that the fermentation process dominated by yeasts in winemaking can promote the residual degradation of tebuconazole. Different yeasts have different degradation effects on tebuconazole. Among the 12 yeasts, the strains D254, RC212, BO213 and AC have better degradation effects of tebuconazole, with a degradation rate of 21%~23%. Tebuconazole significantly changed the aroma components produced during alcohol fermentation, severely inhibits the formation of benzyl alcohol (bitter almond flavor) and destroys the wine flavor structure. Among the 12 kinds of yeast tested, the formation of flavor substances during the fermentation of AC strains is the least affected by tebuconazole. In summary, it is recommended that yeast AC be selected for fermentation in winemaking.
Research progress on detection technology of organophosphorus pesticide metabolites in biological samples
Chenglong ZHANG, Fei GUO, Ruiqin YANG, Peng LI
 doi: 10.16801/j.issn.1008-7303.2021.0070
[Abstract](84) [FullText HTML](54) [PDF 444KB](2)
Abstract:
The detection and analysis of organophosphorus pesticide metabolites play an important role in the determination of organophosphorus pesticide nosotoxicosis and poisoning cases, clinical diagnosis, biological monitoring and so on. The development of accurate detection technology of trace and even ultra trace organophosphorus pesticide metabolites, and the establishment of a method for the detection of organophosphorus pesticide metabolites in complex biological samples have become one of the urgent problems to be solved in forensic science. At present, the common laboratory detection methods at home and abroad include gas chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, etc. This paper focuses on the research progress of these detection technologies, the pretreatment techniques for blood and urine samples such as liquid-liquid extraction, solid-phase extraction and QuEChERS, as well as the pretreatment techniques for hair samples such as the solid-liquid extraction method. In addition, the principle and application progress of fluorescent probe, immunoassay, biosensor and other rapid detection technologies are introduced, and the problems of existing detection technologies are summarized.
Development and application of oxadiazon-fertilizer slow-release granule for synchronous application in mechanical transplanting rice
Wei TANG, Jianping ZHANG, Yongjie YANG, Jing YUAN, Jie CHEN, Yongliang LU
 doi: 10.16801/j.issn.1008-7303.2021.0029
[Abstract](261) [FullText HTML](181) [PDF 477KB](12)
Abstract:
Weed infestation is a serious problem in mechanical transplanting rice in China. Developing pre-emergent (PRE) herbicide-fertilizer slow-release granule and its assorted application technology is one of the most effective way to improve the efficiency. In this work, three types of slow-release oxadiazon-fertilizer granule (SROG) coated with poly-lactic acid with a core-shell structure were developed (contained 0.25% oxadiazon active ingredient). The efficacy and rice safety of SROG were evaluated in mechanical transplanting rice fields. The results indicated that, when transplanting was applied in the same time at 180 kg/hm2 (450 g a.i./hm2 of oxadiazon), the three types of SROG (with different concentration of coating material) disintegrated 3 to 7 days after the application, and had over 90% control efficacy against Echinochloa spp. and Monochoria vaginalis 35 days after transplanting, which were similar to regular PRE application (combined with fertilizer) of oxadiazon EC and pyrazosulfuron-ethyl + simetryne + prometryn WP 5 days after the transplanting. The plant height, aboveground fresh weight and tiller number were greater for the three SROG treatments compare with treatments of the two regular PRE herbicides 35 days after transplanting. Similar weed control efficacy was obtained when the dosage of SROG declined to 80% (144 kg/hm2 or 360 g a.i./hm2). No herbicide injury was observed in all the experiments. The mechanical application of SROG synchronized with the improved side deep fertilizing rice transplanter (just broadcast the SROG on the soil surface) was also systematically investigated. The mechanical transplanting synchronized with SROG application technology could be an effective tool for rice cultivation systems to reduce labor input and herbicide application in the future.
Storage stability of etoxazole in 9 kinds of fruits and vegetables
Zenglong CHEN, Ziqi LIU, Xianjun LIAO, Ziyu YE, Xiaoyu WANG, Wei LI, Dongmei QIN
 doi: 10.16801/j.issn.1008-7303.2021.0061
[Abstract](172) [FullText HTML](106) [PDF 573KB](2)
Abstract:
A gas chromatography/mass spectrometry (GC/MS) method was developed for etoxazole in kiwifruit, papaya, lemon, eggplant, hawthorn, persimmon, sweet pepper, banana and jujube. Then, the storage stabilities and influencing factors of etoxazole were evaluated systematically in above crops at −20 °C for 112 days. The samples were extracted by acetonitrile, purified by aminopropyl solid phase extraction cartridge, and determined by GC/MS. The results showed that the mean recoveries were between 80% and 112%, the relative standard deviations (RSD) were ranged from 1.4% to 12% at the spiking level of 0.01-3 μg/g, and the limit of quantification was 0.01 μg/g. Etoxazole was relatively stable in sweet pepper with degradation rates of 9.0%-28.6%, which were lower than 30%. However, the degradation rates of etoxazole were over 30% in kiwifruit, papaya, lemon, eggplant, hawthorn, persimmon, banana and jujube, demonstrating etoxazole could not be stored stably. The storage stability of etoxazole was closely related to the types of matrix, pH values and water content. Therefore, the samples with etoxazole residues are not recommended to be stored for a long time and should be detected as soon as possible to avoid the deviation of detection results caused by pesticide degradation. This study provided basic data for residue analytical method and storage stability of etoxazole in a variety of fruit and vegetable crops, and also provides reference for accurate quantitation of etoxazole in further studies.
The degradation rules and dietary risk assessment of acetamiprid residues in peach
Xiaolong CHEN, Ya WANG, Jinjin CHENG, Jiangtao ZHAO, Xiangyang YU
 doi: 10.16801/j.issn.1008-7303.2021.0060
[Abstract](191) [FullText HTML](140) [PDF 777KB](6)
Abstract:
Acetamiprid has a high detection rate but is not registered on peach in our country. Lack of information such as application or pre-harvest intervals may lead to irrational pesticide use and high residue risks. In order to identify the residue risks of acetamiprid in peach fruit, degradation experiments and simulated farmer application experiments were carried out. Also, from 2015 to 2018, the acetamiprid residues in peach from nine main producing areas in China were investigated and the dietary intake risk was analyzed. The results showed that the degradation of acetamiprid in peach peel and pulp conformed to the first-order kinetic equation, and the half-lives were 3.92 and 3.14 d, respectively. Simulated farmer application experiments showed that the residual amounts at 7, 14 and 21 d after last application were low in both applications and far lower than the maximum residue limit(MRL), and removing the peach peel can drastically reduce the intake risks. The detection rate in 509 peach samples from the nine producing areas ranged from 8% to 38%, and all the residues did not excess the MRL. The contribution rate of acetamiprid on peaches to the total chronic dietary exposure ranged from 0.02% to 0.07%, which was relatively low and had no unacceptable risk for general population.
Determination of 31 pesticide residues in Chinese chives by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry
Haolin LI, Tongtong LI, Yuying DONG, Lifei HE, Beixing LI, Wei MU
 doi: 10.16801/j.issn.1008-7303.2021.0054
[Abstract](230) [FullText HTML](150) [PDF 356KB](7)
Abstract:
Based on QuEChERS and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), a method for simultaneous detection of 31 pesticide residues in Chinese chives was established. The Chinese chive samples were extracted by acetonitrile, cleaned-up by modified QuEChERS method and then analyzed by UPLC-MS/MS. Results showed that good linear relationship was obtained between the mass concentrations of 31 pesticides and the corresponding peak areas in the range of 0.5-100 μg/L with all of the correlation coefficients higher than 0.995, and the LOQs (Limits of quantification) of the pesticides were all 10 μg/kg. The average recoveries of 31 pesticides ranged from 70%-102% at the spiking level of 0.01, 0.1 and 1 mg/kg with RSDs lower than 11% (n = 5). The method was rapid, simple, reliable, efficient, and low cost, and was suitable for simultaneous determination of 31 pesticide residues in Chinese chives.
Distribution of NPEOs and NP in 4 formulations of abamectin and their migration from packing
Huili LUO, Xiaomei HE, Jingru ZHOU, Gefan ZHANG
 doi: 10.16801/j.issn.1008-7303.2021.0062
[Abstract](171) [FullText HTML](104) [PDF 604KB](2)
Abstract:
The detection of nonylphenol ethoxylates (NPEOs) and nonylphenol (NP) in abamectin pesticide formulations was conducted using high performance liquid chromatogram-fluorescence method, and distribution characteristics of NPEOs and NP in 4 formulations: emulsifiable concentrate (EC), microemulsion (ME), emulsion in water (EW), suspension concentrate (SC) were analyzed. Solution migrations of NPEOs and NP from outer packing material (plastic) were detected by soaking the samples with methanol as an oil-based analog, and the sources of NPEOs and NP in pesticide formulations were analyzed. Results showed that the detection rate of NPEOs, NP, and both in the 4 formulations was 60.47%, 62.79%, 51.16%, respectively. The detection of NPEOs and NP in complexation agent was higher than that in a single agent. The mean and median value of NPEOs and NP in 4 formulations from high to low both were EC > EW > ME > SC. Among them, EC contained 6.83% of NPEOs and 8.41% of NP, both were the highest in the tested samples. Component of NPEOs was more than that of NP in EC, while both were used equally in EW. 2 h migrations of NPEOs and NP were 0.16-49.34 and 0.19-18.05 µg/cm2, respectively, while the values after 30 days were 0.76-66.48 and 2.84-137.79 µg/cm2, respectively. At the beginning of the experiment, migration of NPEOs was more stable than NP, but migration of the both were close at 15 d, which ranged from 46.64%-100.82% and 46.89%-102.03% of 30 d migrations. The highest contribution of NP from outer packing plastic was 2.43%, while it was 0.241% for NPEOs. 30 d contribution of NP was 1.66-107.51 times to that of NPEOs, and the contribution of NP from plastic bags was higher than that from plastic bottles. The results demonstrated that NP was used more often than NPEOs in the outer packing of pesticide, but additives during production was the main source of NPEOs and NP in pesticide.
Effects of different auxiliaries, spray nozzles and spray pressures of self-propelled boom sprayer on spray effect in paddy filed
Rui YANG, Xiang XU, Xuegui WANG, Changwei GONG, Yunzheng ZHANG, Yanwei RUAN, Debin YANG, Xudong YANG
 doi: 10.16801/j.issn.1008-7303.2021.0035
[Abstract](12) [FullText HTML](9) [PDF 726KB](2)
Abstract:
In this study, the effects of six spraying auxiliaries(Red Sun, Pele, Maisi, Rongtou, Neem Oil and Hasuteng), three types of spray nozzles(TEEJET-VP80015, ASJ-VP110015 and LICHENG-VP11003) and three types of spraying pressures(0.2, 0.4, 0.6 MPa) on pesticide utilization rate of deposition, the atomization performance (D50, droplet density, et al), spray droplet distribution uniformity and the control efficiency of 240 g/L thifluzamide SC on rice sheath blight disease and rice yields were studied by YIFENG-MARUYAMA 3WP-500CN self-propelled boom sprayer in field test and using the Allura Red AC 85 as an indicator. The results indicated that the spray droplet distribution uniformity of Hasuteng was significantly higher than that of other auxiliaries under the condition of the TEEJET-VP80015 nozzle and 0.4 MPa spray pressure, which of the coefficient of variation reached 0.11, meanwhile the effects on the estimated deposition of droplets(45.74 μL/cm2) and span of distribution(1.29) were significantly higher than those of other auxiliaries; The effect of auxiliary Maisi on the density of droplets(103.78 droplet/cm2) and utilization rate of pesticide deposition(83.88%) were significantly higher than those of other auxiliaries. Different pressures using the TEEJET-VP80015 nozzle had significant effect on span of distribution, adherence rate of droplets and utilization rate of pesticide deposition without auxiliaries, and the span of distribution, the adherence rate of droplets and the utilization rate of pesticide deposition reached 1.18, 33.32%, and 78.19% respectively when the pressure was set for 0.6 MPa. When without auxiliaries and under the condition of 0.4 MPa, the LICHENG-VP11003 nozzle displayed a greater influence on the spray droplet distribution uniformity, and was significantly higher than that of the other two nozzles, which of the coefficient of variation was 0.12, had a greater impact on the coverage (69.37%), estimated deposition of droplet(42.77 μL/cm2) and utilization rate of pesticide deposition (75.79%) were significantly higher than those of the other two nozzles. The effect of control efficacy of 240 g/L thifluzamide SC on the rice sheath blight disease was consistent with the results of the performance and atomization quality of deposition droplets. The control efficiency of adding the auxiliary Maisi on sheath blight was significantly higher than that of adding other auxiliaries, reached 89.27%.When increasing the spray pressure to 0.6 MPa, the control efficiency was promoted to 88.67%, which was significantly higher than other pressures. When using TEEJET-VP80015 nozzle and under the conditions of 0.4 MPa spray pressure, the rice yield reached 8301 kg/hm2, which was significantly higher than artificial spraying. Therefore, the auxiliaries and the spray nozzles have produced a significant impact on the utilization rate of pesticide deposition, uniformity of the droplets, atomization quality of deposition droplets of self-propelled boom sprayer, and the control efficiency of pesticides can be improved by adding auxiliaries under appropriate spray pressure.
Study on the deposition, degradation and minimum effective dose of azoxystrobin in soybean
Zhou TONG, Mingna SUN, Yue CHU, Dongqiang HU, Xu DONG, Mei WANG, Tongchun GAO, Jinsheng DUAN
 doi: 10.16801/j.issn.1008-7303.2021.0066
[Abstract](71) [FullText HTML](50) [PDF 494KB](3)
Abstract:
Azoxystrobin is an important chemical to control soybean rust, it is an urgent task to clarify the residue rule of azoxystrobin in soybean. In this study, ultra performance liquid chromatography tandem mass spectrometry was used to establish a method for the determination of stems, leaves, pods and soil residues in soybean planting system, the detection limit was 0.005 mg/kg. The results of field experiment showed that azoxystrobin 250 g/L SC was mainly deposited in soybean leaves after application and decreased gradually from north to south, the degradation rate was faster in the upper stems and leaves and no significant difference between regions; the relationship between the control effect of azoxystrobin on soybean rust was compared under different doses, the residue was provided, and minimum effective dose of azoxystrobin was obtained 225 g a.i /hm2. The research results of this paper have important significance to guide the scientific application of azoxystrobin in soybean production, and then help the practice of pesticide reduction on soybean.
Research progress of gelatin microspheres
Qizhen ZHANG, Mingming YIN, Manli YU, Fuliang CHEN
 doi: 10.16801/j.issn.1008-7303.2021.0068
[Abstract](168) [FullText HTML](47) [PDF 686KB](9)
Abstract:
Currently, the excessive use of traditional pesticide formulations has resulted in a series of environmental pollution and ecological hazard due to their poor utilization and short-term effectiveness. Thus, development of effective, safe and controlled-release pesticide formulations would offer great benefits to the sustainable agriculture. Gelatin is a natural polymer material. Because of its nontoxicity, abundant supply, biodegradable and good film -forming properties, gelatin has become an excellent carrier for controlled release of active ingredients in biology, medicine and pesticide. This paper reviewed the recent research progress of gelatin microspheres, especially their advantages and disadvantages in different preparations. The chemical modification by a large number of active groups to the molecular structure of gelatin microspheres was also summarized. Finally, major challenges in drug-loaded gelatin microspheres for medical application and prospects for pesticide development were also analyzed. This study is expected to contribute in providing some theoretical and technological references in promoting the development of gelatin microspheres for agriculture utilizations.
Sensitivity baseline to boscalid of Alternaria alternata causing tobacco brown spot in Guizhou Province
Feibin LEI, Hancheng WANG, Yuanfeng DAI, Chuanqing ZHANG
 doi: 10.16801/j.issn.1008-7303.2021.0064
[Abstract](93) [FullText HTML](58) [PDF 529KB](5)
Abstract:
The pathogenic fungus causing tobacco brown spot in Guizhou Province was isolated and identified from diseased samples collected during 2014 to 2015 from where succinate dehydrogenase inhibitors have never been used, and their sensitivity baseline to boscalid was established by mycelial growth rate tests. There were significant differences in colony and conidium morphlogy, and pathogencicity among these isolates, however, all isolates were identified as Alternaria alternata. The EC50 values of boscalid inhibiting growth of A. alternata population (n = 102) from tobacco fitted unimodal distribution and varied from 0.186 to 5.818 μg/mL with the mean value of (2.157 ± 1.112) μg/mL, which could be adopted as the baseline sensitivity of A. alternata on tobacco to boscalid and used for monitoring the sensitivity shift in future. Further study indicated that there was some nucleotide polymorphism in codons, such as 209, 277 and 224 in SdhB of A. alternata. However, no relationship was observed between this nucleotide diversity and the sensitivity to boscalid in A. alternata causing tobacco brown spot.
Research progress in chromatographic separation of triazole pesticides containing two chiral centers
Shouying TANG, Fei WANG, Xiurou MENG, Yuping ZHANG
 doi: 10.16801/j.issn.1008-7303.2021.0065
[Abstract](118) [FullText HTML](75) [PDF 527KB](5)
Abstract:
Triazole fungicides are widely used fungicides in the world. The vast majority of triazole fungicides are chiral pesticides with one or two chiral centers and two or four enantiomers. Based on the research results of triazole fungicides in recent years, this article summarized the chromatographic methods such as high performance liquid chromatography, supercritical fluid chromatography, capillary electrophoresis, gas chromatography, and convergence chromatography for the chiral analysis of 11 triazole pesticides with two chiral centers including epoxiconazole, paclobutrazol, triadimenol, bitertanol, propiconazole, difenoconazole, metconazole, diclobutrazol, cyproconazole, bromuconazole, and etaconazole. The research progress in the separation and determination of triazoles with different chiral centers can provide references for the separation, analysis, and in-depth study of triazole compounds with multiple chiral centers.
Review on uptake and translocation behaviors of pesticides in plants and application technologies of pesticides
Tingting LIU, Shangke LIU, Beixing LI, Feng LIU, Wei MU, Canping PAN, Nan ZOU
 doi: 10.16801/j.issn-1008-7303.2021.0067
[Abstract](153) [FullText HTML](125) [PDF 612KB](11)
Abstract:
The application methods and application efficacy of pesticide is closely related to their uptake and translocation behaviors in the plants. The uptake and translocation behaviors of pesticides on the surface and inside of plants are not only related to the physical and chemical properties of pesticides, but also affected by some factors, such as plants species, plants growth period, growth conditions and application technologies. The uptake and translocation of pesticides in plants and the influencing factors have important guiding significance for the selection of application technologies and the improvement effective utilization of pesticides. This article reviews the uptake and translocation behaviors of pesticides in the plants, the relationship between conduction modes and application technologies of pesticides, and the factors influencing the uptake and translocation behaviors of pesticides and measures to improve the uptake and translocation behaviors of pesticides were also proposed, in order to provide some theoretical support for the safe and reasonable application of pesticides.
Antifungal activity of compound 1S,2R-((3-bromophenethyl)amino)-N-(4-chloro-2-trifluoromethylphenyl) cyclohexane-1-sulfonamide against Botrytis cinerea and its mode of action
Jingnan PENG, Huazhong ZHANG, Changle LI, Xinghai LI, Zhiqiu QI
 doi: 10.16801/j.issn.1008-7303.2021.0055
[Abstract](182) [FullText HTML](106) [PDF 486KB](4)
Abstract:
The antifungal activity of sulfonamide compound 1S, 2R-((3-bromophenethyl)amino)-N-(4-chloro-2-trifluoromethylphenyl)cyclohexane-1-sulfonamide (SYAUP-CN-26) against Botrytis cinerea and its mode of action for controlling diseases were studied. The results showed that SYAUP-CN-26 could inhibit hyphal growth and spore germination of some plant pathogenic fungi, especially for B. cinerea with the EC50 value of 1.82 μg/mL and 14.98 μg/mL. The spore production, sclerotic production and single sclerotic weigh were reduced significantly under the treatment of 20 μg/mL of SYAUP-CN-26. The pathogenicity of B. cinerea treated by SYAUP-CN-26 was significantly lower than that of the control. SYAUP-CN-26 at 200 μg/mL provided control efficacies of 83.11% and 47.5% for protective and curative spraying against tomato gray mold, respectively. Therefore, it showed that SYAUP-CN-26 possessed better protective activity than curative activity.
Display Method:
2021, 23(2): 1-1.  
[Abstract](94) [FullText HTML](81) [PDF 166KB](21)
Abstract:
2021, 23(2): 1-1.  
[Abstract](75) [FullText HTML](68) [PDF 397KB](10)
Abstract:
2021, (2): 1-4.  
[Abstract](79) [FullText HTML](69) [PDF 443KB](14)
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MONOGRAPHS AND REVIEWS
Research progress on chemical synthesis and application of the sex pheromone of Spodoptera frugiperda
Xiao SUN, Yanhua WU, Min WANG, Qinghua BIAN, Jiangchun ZHONG
2021, 23(2): 199-208.   doi: 10.16801/j.issn.1008-7303.2021.0042
[Abstract](436) [FullText HTML](234) [PDF 1639KB](50)
Abstract:
Sex pheromone is one of the most promising and environment-friendly strategies to control the fall armyworm moth. In this review, the separation process, structure identification and application of the sex pheromone of Spodoptera frugiperda were summarized. Its compoments comprise monoolefinic esters and diolefinic esters. The chemical synthesis of the sex pherpmone were reviewed. Among them, the construction of the Z- double bond was mainly involved in catalytic hydrogenation of alkyne, Z-selective cross metathesis of olefin, Z-olefin, Wittig coupling, vinylic organoborane and ring opening of cyclooctadiene and the E-one included Grignard coupling, ring opening of cyclepropylethanol and E-olefinic ester. Besides, the current problems and the future researches of the sex pheromone of S. frugiperda were discussed.
Advances in structures and inhibitors of trehalose synthetase
Zhiyang JIANG, Qing HAN, Jin'e WANG, Kai ZHU, Jingyu ZHANG, Mingfei DENG, Jiaxing HUANG, Hongxia DUANG
2021, 23(2): 209-225.   doi: 10.16801/j.issn.1008-7303.2021.0043
[Abstract](510) [FullText HTML](410) [PDF 1759KB](48)
Abstract:
Trehalose is a non-reducing disaccharide, which exists widely in nature and possesses important biological functions. It is not only an energy storage substance participating in energy metabolism, but also a structure substance participating in the formation of fungal cell walls and insect exoskeletons. Meanwhile, trehalose can regulate the pathogenicity of pathogens, and the growth and development of insects. Trehalose synthetase is mainly responsible for catalyzing the biosynthesis of trehalose, which includes two functional domains: trehalose-6-phosphate synthetase and trehalose-6-phosphate phosphatase. More and more recent studies showed that trehalose synthetase has a great potential as a novel target of pesticides. This review summaried the protein crystal structures, substrate binding modes, and chemical structures of reported inhibitors for trehalose-6-phosphate synthetase and trehalose-6-phosphate phosphatase. It is expected to provide guidance for the screening of inhibitors, the design and the modification of lead compounds, and the development of new pesticides targeting trehalose synthetase in the future.
Comparison and analysis on the maximum residue limits for plant growth regulators in foodstuffs
Wen SONG, Qiang WANG
2021, 23(2): 226-236.   doi: 10.16801/j.issn.1008-7303.2021.0012
[Abstract](119) [FullText HTML](79) [PDF 1121KB](16)
Abstract:
The usage and maximum residue limits (MRLs) for plant growth regulators (PGRs) in foodstuffs are social issues widely concerned by the public and various stakeholders. This paper overviews the latest updates on PGRs in the Chinese national food safety standard, MRLs for pesticides in foods (GB 2763—2019), and conducted a matching analysis with domestic PGR registration and application. Furthermore, the PGR MRLs among China, Codex Alimentarius Commission (CAC), USA, Japan and EU were compared. The main findings and suggestions were given in this review. Firstly, the domestic standard covers almost half (41.7%) registered PGR active ingredients, which surpasses CAC. Secondly, the domestic standard basically contains staple crops, but the product categories and their classification stipulated in the standard are not as rich and detailed as those in EU and Japan. Especially for minor crops and foodstuffs of animal origin. The standard system for PGRs still needs to be further improved. Thirdly, the domestic standard is not aligned to international standards in some extent, and may have less influence on international trade. Finally, suggestions were put forward to improve the MRL standard system of PGRs, such as synchronising the MRL standard with the pesticide registration, and acting on the international convention.
Current situation on classification of medicinal crops based on pesticide residues
Yanjie LI, Changpeng ZHANG, Xianjun LIAO, Xueping ZHAO, Fugen LI
2021, 23(2): 237-244.   doi: 10.16801/j.issn.1008-7303.2021.0053
[Abstract](360) [FullText HTML](193) [PDF 423KB](31)
Abstract:
The situation of pesticide registration and maximum residue limit (MRL) establishment of medicinal crops in China and the classification of medicinal crops in China and abroad were summarized. Suggestions on the classification of pesticide residue test groups and the selection of representative crops were proposed. These are of great significance for accelerating pesticide registration and MRL establishment for medicinal crops, improving the quality and safety of medicinal crops, and promoting the industrial development.
Research progress on the synergistic regularity and application of spray adjuvants on the foliage-applied herbicides
Zilu LI, Chenhui ZHANG, Yongfei GUO, Zhongli LU, Yuxia GAO, Fengpei DU
2021, 23(2): 245-258.   doi: 10.16801/j.issn.1008-7303.2021.0044
[Abstract](529) [FullText HTML](305) [PDF 1023KB](53)
Abstract:
Weeds affect the agricultural production and development seriously. Chemical control with herbicide is the most time-saving, labor-saving and high-efficiency weed control method at present. Among them, foliage-applied herbicides are widely used because they are hardly affected by soil environment and applied according to weeds, which exhibits high flexibility and selectivity. However, herbicides droplets often splash, roll off, and penetrate difficultly as a result of the unique interfacial characteristics of weed leaf during the spraying process, causing overuse of herbicides, herbicide resistance, phytotoxicity and environmental residue, etc. Adding appropriate spray adjuvants is an effective strategy to solve the above problems. Considering that the application of herbicides should be combined with the weeds and spray adjuvants, it is of great significance to understand their respective action modes for guiding weeds control. This review first introduces the mode of action and application of herbicides, then summarizes the morphological and foliar interfacial characteristics of gramineous weeds, broadleaf weeds and cyperaceous weeds and their influences on herbicide selection. Moreover, the synergistic mechanism of commonly used spray adjuvants on folliage-applied herbicides and the influence of adjuvants on dose transfer process are also elucidated in detail. On this basis, the mechanism and application of spray adjuvants on contact herbicides and translocated herbicides for controlling gramineous weeds, broadleaf weeds and cyperaceous weeds are summarized. In addition, the future development of herbicide spray adjuvants is also prospected, aiming to provide references for the development and application of spray adjuvants in the field of herbicides, and finally achieving the goal of "reducing dosage and increasing efficiency".
Potential applications of copper-based nanoparticles in pesticide
Xinxin DONG, Yanfei JI, Ye TIAN, Jie ZHANG, Chengwei LIU
2021, 23(2): 259-268.   doi: 10.16801/j.issn.1008-7303.2021.0015
[Abstract](124) [FullText HTML](131) [PDF 725KB](28)
Abstract:
Copper-based nanoparticles are one of the most frequently prepared and used nanomaterials in industry. They have the characteristics of large specific surface area, high activation energy and many active sites, which have wide application prospect. Copper-based nanoparticles can improve the nutritional absorption and growth parameters of plants, and induce systemic resistance. Therefore can be used as plant growth regulators. In addition, copper nanoparticles also have physiological toxicity, which can cause oxidative stress reaction and membrane disintegration in cells. This property can be used in the field of pesticide as antimicrobials or herbicide. This review summaried the research progress of the growth promoting mechanism of copper-based nanoparticles and the physiological damage in cells and their related mechanism. The potential application of copper-based nanoparticles as plant growth regulators, antimicrobials and herbicides in the field of pesticide was discussed. And this review has also provided new ideas for the research and production of new pesticides.
RESEARCH REPORTS
Synthesis and biological activities of novel triazole piperzazine derivatives
Shenchuan DENG, Xujun LI, Xiang ZHU, Xiaoying DU, Junkai LI, Zhihong XU
2021, 23(2): 269-278.   doi: 10.16801/j.issn.1008-7303.2021.0009
[Abstract](881) [FullText HTML](426) [PDF 488KB](51)
Abstract:
Twenty novel triazole piperzazine derivatives 7a - 7t were synthesized using 1,2,4-triazol, 2-chloro-1-(2,4-difluorophenyl) ethanone and piperzazine compounds as the starting materials, through the combination of active substructures. All target compounds were characterized by 1H NMR, 13C NMR and HRMS. The fungicidal activities and insecticide activities of compounds were evaluated by the hyphal growth rate method and the drop method. The results showed that most of those compounds exhibited high inhibitory effects against Rhizoctonia solani, Fusarium graminearum and Magnaporthe oryzae. Compounds 7n , 7r and 7s exhibited good fungicidal activities with the inhibition rate of 60.19%, 62.27% and 50.00% against F. graminearum at the concentration of 200 μmol/L, resepectively. They were equal to triadimenol. And the EC50 value of compound 7r was 49.49 μmol/L against R. solani. Moreover, The results indicated that compound 7o showed 40.00% mortality rate against Spodoptera litura larva at 100 mg/L, which was slightly lower than that of the commercial insecticide cyhalothrin (46.67%). The compounds with good fungicidal activities and insecticidal activities were synthesized in this work, which provided a reference for the activity study for novel triazole piperzazine derivatives.
Synthesis and biological activity of avermectin derivatives containing hydrazide structure
Zechun WANG, ALan WEI, Jiao LI, Fengbo XU
2021, 23(2): 279-286.   doi: 10.16801/j.issn.1008-7303.2021.0004
[Abstract](305) [FullText HTML](178) [PDF 582KB](28)
Abstract:
To reduce energy consumption and environmental pollution and improve the practical application value of abamectin B2, the 23-OH was reacted with pyridine formylhydrazide, benzene sulfonyl hydrazide, brominated benzoylhydrazide and hydrazide formate after oxidized to carbonyl. Six avermectin derivatives with hydrazide structure were designed and synthesized. New compounds were confirmed by HMRS and 1H NMR and were preliminarily tested its insecticidal and acaricidal activities against diamondback moth, aphid and vermilion leaf mites. The insecticidal activities of target compounds indicated that the mortality rates of avermectin B2a with m-bromobenzoyl hydrazine and isonicotinic hydrazine against diamondback moth at 1 μg/mL were 75% and 50%, respectively, which were significantly higher than those of benzene sulfonyl hydrazide and methoxy formyl hydrazine abamectin B2a derivatives, respectively.
Development of anti-thiamethoxam full-length recombinant antibody and investigation of the specific recognition mechanism
Pengyan LIU, Yuanhao GUO, Shasha JIAO, Yang CHEN, Yirong GUO, Guonian ZHU
2021, 23(2): 296-307.   doi: 10.16801/j.issn.1008-7303.2021.0008
[Abstract](893) [FullText HTML](358) [PDF 1323KB](20)
Abstract:
In this study, the recombinant antibody against thiamethoxam was prepared and the specific molecular recognition mechanism between the antibody and thiamethoxam was studied via computer-assisted homology modeling and molecular docking. Firstly, surface plasma resonance (SPR) technique was used to evaluate the recognition features of monoclonal antibody (mAb) against thiamethoxam. Secondly, the specific variable regions of heavy and light chains (VH and VL) in anti-thiamethoxam mAb were amplified from a hybridoma cell line, and full-length recombinant antibody (rAb) was successfully in vitro expressed by mammalian cell HEK 293 (F). At last, the molecular recognition mechanism of the antibody’s high specificity and sensitivity to thiamethoxam was investigated by homology modeling and molecular docking, based on the correct sequences of VH and VL. The results showed that the mAb could specifically recognize thiamethoxam and had a high binding affinity with dissociation equilibrium constant KD of 7.995 × 10−11 mol/L. As evaluated by indirect competitive enzyme-linked immunosorbent assay (ic-ELISA), the performance of full-length rAb was similar to that of the parental mAb, exhibiting high specificity and high sensitivity to thiamethoxam, with the IC50 value of 0.41 μg/L to thiamethoxam. No cross reactivity to other neonicotinoid pesticides was observed (< 0.04%). The results demonstrated that Asn39 (L-CDR1) and the other 8 amino acid residues in the hydrophobic binding pocket interacted with the target mainly through hydrogen bond and van der Waals, which appeared to be the predominant contributor to the selectivity (specificity) of the antibody. His35 (H-CDR1) and Trp108 (H-CDR3) residues located in the VH affected on the binding affinity of the antibody against thiamethoxam. In conclusion, the full-length rAb prepared in this study can replace traditional monoclonal antibody as the core reagent to establish a variety of immunoassay methods for the detection of thiamethoxam residues in environmental samples and agricultural products. The study of the recognition mechanism can provide theoretical guidance for the further improvement of antibody affinity.
Insecticidal activity of periplocosides against oriental armyworm (Mythimna separata) and its effects on three characteristic enzyme activities in the midgut cell BBMV
Mingxing FENG, Zhaonong HU, Wenjun WU
2021, 23(2): 308-315.   doi: 10.16801/j.issn.1008-7303.2021.0003
[Abstract](284) [FullText HTML](181) [PDF 597KB](24)
Abstract:
The toxicity of six periplocoside compounds against 3th M. separata larvae was measured by toxic carrying leaf disc method, the activities of aminopeptidase, alkaline phosphatase and V-ATPase in BBMV were determined using six periplocoside compounds on the basis of preparing brush border membrane vesicles (BBMV) of oriental armyworm midgut cells by MgCl2 precipitation and differential centrifugation. The results showed that PSP and PST had obvious insecticidal activity with LC50 value of 1.60 and 1.23 mg/mL at 24 h, respectively. PSA, PSD and PSF revealed weak insecticidal activity (LC50 > 20 mg/mL) while PSE had no insecticidal activity. Six periplocosides had no significant inhibitory effect on aminopeptidase and alkaline phosphatase. The activity of V-ATPase was significantly inhibited by PSP and PST with a concentration dependence manner. Therefore, we preliminarily speculated that the initial binding site of insecticidal periplocoside compounds was located on the V-ATPase.
Regulation of pakchoi's secondary metabolites on the behavior of female Plutella xylostella (Lepidoptera: Plutellidae)
Zhandi WANG, La ZHANG, Bailian DING, Yundong SHI, Yani WANG, Guangqiu LU, Lin JIA
2021, 23(2): 323-330.   doi: 10.16801/j.issn.1008-7303.2021.0016
[Abstract](206) [FullText HTML](115) [PDF 789KB](22)
Abstract:
To clarify the regulation of pakchoi’s secondary metabolites on the behavior of Plutella xylostella L., Various polar substances from pakchoi using the heat reflux method were extracted. The regulation of these substances on the behavior of female P. xylostella was evaluated with a Y-tube olfactometer, and the chemical structures in the extract were identified by GC-MS. The results showed that all the extracts with varying polarities of pakchoi regulated the behavior of female P. xylostella. The low-polarity substances attracted females at high concentrations, and the high-polarity substances lured females at medium and low concentrations. Comparing the anhydrous-ethanol extracts with the distilled-water extracts of pakchoi, the former had lower attractant activity to P. xylostella than the latter at low concentrations. The results of GC-MS identification showed that the distilled-water extracts of pakchoi contained two compounds, namely ethyl iso-allocholate and 9,12,15-octadecatrienal, among which the concentration of ethyl iso-allocholate was higher. The anhydrous-ethanol extracts of pakchoi contained six compounds, the substance with the highest concentration was 3,7,11,15-tetramethyl-2-hexadecen-1-ol, followed by 9,12,15-octadecene carbtrienoic acid, in which 9,12,15-octadecatrienic acid and 9,12,15-octadecatrienal had the same parent ring structure. The results showed that 9,12,15-octadecatrienic acid and 9,12,15-octadecatrienal were the substances with potential activities to regulate the behavior of P. xylostella on pakchoi, which could be used for the development of lead compounds for the green control of P. xylostella.
Influencing factors of dipping seedling dip with thiophanate-methyl and chlorothalonil against the black rot of sweet potato
Desheng ZHANG, Ruiying BAI, Qi QIAO, Yuting TIAN, Yongjiang WANG, Shuang WANG, Zhenchen ZHANG
2021, 23(2): 331-340.   doi: 10.16801/j.issn.1008-7303.2021.0034
[Abstract](469) [FullText HTML](232) [PDF 697KB](28)
Abstract:
In this work, the effects of different factors on the infection of black rot of sweet potato seedlings were investigated and the necessity of optimizing seedling dip technology according to the types of fungicides was studied. Thiophanate-methyl with internal absorption activity and chlorothalonil without internal absorption activity were used in our experiments. Firstly, the control efficiencies on black rot of sweet potato seedlings using different dipping time and pesticide concentrations were determined, respectively. Secondly, the orthogonal experiments were conducted to envaluate the effects of dipping time, treatment concentration and spore concentration by measuring the disease index. Thirdly, the relationship between the dipping conditions and the control efficiencies was explored by the combination experiments of the dipping time and the treatment concentration. Finally, the control efficiencies of dipping seedlings were verified by the experiments in the disease nursery. When the dipping time was less than 6 h for the thiophanate-methyl group and less than 3 h for the chlorothalonil group, the control efficiencies against black rot of sweet potato seedlings increased with the dipping time. Similarly, When the treatment concentrations were less than 600 mg/L for the thiophanate-methyl group and less than 700 mg/L for the chlorothalonil group, their control efficiencies increased with the treatment concentrations. For the thiophanate-methyl group, the effects of spore concentration, dipping time and the pesticide concentration on the occurrence of disease were weakened successively. Whereas, for the chlorothalonil group, the effects of spore concentration, pesticide concentration and dipping time on the occurrence of disease were weakened successively. All three factors had significant effects on the occurrence of disease. The gap of control efficiencies between 700 mg/L and 400 mg/L of thiophanate-methyl widened with dipping time, and the maximum value was 26.8%. The gap of control efficiencies between 360 min and 30 min widened with concentration, and the maximum value was 42.8%. However, similar trends were not observed in test results of the chlorothalonil group. In the disease nursery, the control efficiencies of thiophanate-methyl and chlorothalonil treatment for 6 h were 83.6% and 85.2%, respectively. And the corresponding fresh weights were 60.1 g and 58.8 g, respectively. The performance of those two treatments were significantly better than others. However, when the dipping time was decreased to 2 h or 10 min, the control efficiencies of the chlorothalonil group were significantly higher than those of the thiophanate-methyl group, which were consistent with the pot experiments. Dipping time, pesticide concentration and spore concentration are the key factors which affect the control efficiency. The influences of each factor on the occurrence of disease vary with the type of the fungicide. The required dipping time of the thiophanate-methyl group is significantly higher than that of the chlorothalonil group. Different types of fungicides need to be matched with the corresponding dipping technology to ensure the control efficiency.
Isolation and identification of pathogen causing anthracnose on Zinnia elegans Jacq. and fungicides screening
Wen LI, Yueqiu HE, Jiaying WANG, Guoliang WANG, Zhilong WANG
2021, 23(2): 341-347.   doi: 10.16801/j.issn.1008-7303.2021.0017
[Abstract](706) [FullText HTML](359) [PDF 587KB](29)
Abstract:
To clarify the pathogen of anthracnose on Zinnia elegans Jacq., according to Koch's law, the diseased leaves were collected for the pathogen isolation and pathogenicity testing. After the pathogenicity test, based on their morphologic characteristics, the isolates were proved to be closely related to Colletotrichum species. To further investigated the pathogen, molecular identification based on the phylogenetic analysis of ACT (actin gene), CHS (chitin synthase A gene), GAPDH (glyceraldehyde-3-phosphate dehydrogenase), ITS (ribosomal internal transcribed spacer), SOD2 (manganese-superoxide dismutase), GS (glutamine synthatase), CaM (calmodulin) and TUB2 (beta-tubulin) was conducted and the pathogen was identified to be C. siamense. Furthermore, the antibiotic activity of nine fungicides to this pathogen was tested in vitro and it was found that the EC50 values of trifloxystrobin + tebuconazole 75% water dispersible granule (WG), triflumizole + tebuconazole 35% suspension concentrate (SC), chlorothalonil 75% wettable powder (WP), azoxystrobin 250 g/L SC, prochloraz 50% WP, difenoconazole 10% WG, prothioconazole 10% SC, fluazinam 500 g/L SC and bromothalonil 25% WP were 0.152, 0.407, 2.48, 252, 0.0342, 0.556, 317, 0.00291 and 27.4 mg/L, respectively. Among them, fluazinam 500 g/L SC and prochloraz 50% WP showed the strongest fungicidal activities.
Study on the enantioselectivity cytotoxicity and oxidative damage of hexaconazole on MCF-7 cells
Yang LAN, Dali SUN, Junxiao PANG, Xiaohong SUN
2021, 23(2): 348-356.   doi: 10.16801/j.issn.1008-7303.2021.0020
[Abstract](439) [FullText HTML](246) [PDF 1118KB](16)
Abstract:
In this work, the enantioselective toxicity and oxidative stress of hexaconazole on MCF-7 cells were investigated.. The activities of MCF-7 cells were tested after the exposure of hexaconazole enantiomers by CCK-8 kit. The changes of LDH release, ROS production, SOD and CAT enzyme activities were measured by oxidative damage kits. Results showed that cell activities decreased from 85.24%, 87.11% and 103.87% to 4.07%, 5.11% and 5.24%, respectively, after the treatment of (−)-, (+)- and rac-hexaconazole in the range of 10-160 mg/L. (−)-Hexaconazole exhibited the highest inhibitory rate on MCF-7 cell activity, followed by (+)- and rac-hexaconazole. Oxidative damage results showed that after hexaconazole exposure at the concentrations of 20, 40 and 80 mg/L, the intracellular LDH release and CAT enzyme activity were gradually increased with the increase of the concentration, while ROS production and SOD activity were increased first and then decreased with the increase of the concentration. Similar to cytotoxicity results, (−)-hexaconazole induced the highest cell oxidative damage. In conclusion, the toxicity order to MCF-7 cells was (−)-hexaconazole > (+)-hexaconazole > rac-hexaconazole. The results of this study provided a basis for further exploring the cytotoxicity mechanism of hexaconazole and the food safety risk assessment.
Toxicokinetics of 2-bromo-4-fluoroacetanilide in male SD rat
Difeng ZHU, Zhenxuan TONG, Yanwen HONG, Chao CHEN, Jianlan ZHAO, Li PING
2021, 23(2): 357-365.   doi: 10.16801/j.issn.1008-7303.2021.0057
[Abstract](61) [FullText HTML](65) [PDF 672KB](6)
Abstract:
2-Bromo-4-fluoroacetanilide (BFAA) is an intermediate in the synthesis of many N-phenylamides and an important impurity in the synthesis of pesticides. An ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for the rapid and specific determination of BFAA in rat plasma, tissue, urine and feces to obtain the toxicokinetic information of absorption, distribution and excretion of the compound. Plasma and different tissue samples of rats were obtained and processed by protein precipitation method after intragastric and intravenous administration with different doses of BFAA, and the validated UPLC-MS/MS method was used for detection. The absorption toxicokinetic parameters such as the peak time (tmax), the peak plasma drug concentration (Cmax) and the area under the drug concentration-time curve (AUC(0-t)), and bioavailability of BFAA were calculated. And the tissue distribution and excretion characteristics of urine and feces were investigated. The results of plasma toxicokinetic studies indicated that the drug was rapidly absorbed after intragastric administration, and the tmax value of the plasma concentration of BFAA was (0.2 ± 0.1), (0.4 ± 0.2) and (0.5 ± 0.3) h after given at 200, 500 and 1000 mg/kg, respectively. The Cmax and AUC(0-t) value were (32.4±5.0), (45.2±1.8), (38.5±3.2) mg/L and(121.2±40.9), (393.3±51.1), (321.9±38.0) (mg/L)·h, respectively. The bioavailability (F) of BFAA reached 34.1%-83.3%, and the plasma drug time curve had a double-peak phenomenon. It is speculated that there may be reabsorption or intestinal-hepatic circulation in animals. The results of tissue distribution studies showed that BFAA was widely distributed in the tissues and mainly distributed in small intestine, stomach and adipose tissue. In addition, a small fraction of BFAA was found in the brain and testis which indicated that the compound could cross the blood-brain barrier and testicular barrier. BFAA was eliminated in most tissues within 24 hours which indicated that there was no accumulation of the compound. The target distribution coefficient study suggested that BFAA has no obvious selectivity for tissues. Excretion through urine and feces mainly occurred within 0 to 48 hours, accounting for 93% and 92% of total excretion, respectively. The total excretion amount in urine and feces is (80.6 ± 29.8) μg, which only accounts for (0.03 ± 0.01) %, suggesting that the excretion in urine and feces is not the main elimination way of BFAA prototype compound in vivo.
Residue behavior and dietary risk assessment of bifenthrin, thiamethoxam and clothianidin in wheat
Ying LYU, Yanli QI, Pengcheng REN, Shaobo LIAN, Xia WANG, Shu QIN
2021, 23(2): 366-372.   doi: 10.16801/j.issn.1008-7303.2021.0052
[Abstract](131) [FullText HTML](102) [PDF 522KB](14)
Abstract:
A high efficient and simple method for residue analysis of bifenthrin, thiamethoxam and its metabolite clothianidin in wheat and straw was developed. The samples were extracted with acetic acid-acetonitrile, purified with anhydrous magnesium sulfate, primary secondary amine (PSA) and GCB, and detected by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS). The results showed that there was a good linear relationship between the peak areas of bifenthrin, thiamethoxam and clothianidin and their mass concentrations in the range of 0.002 5-0.1 mg/L, with R2 greater than 0.99. The recoveries of bifenthrin, thiamethoxam and clothianidin in wheat and straw were 93%-98%, 87%-98% and 87%-98%, respectively, and the relative standard deviations (RSDs) were 0.8%-4.8%, 0.6%-4.1% and 1.0%-3.3%, respectively, when the spiked levels were 0.01, 0.1, 0.5 mg/kg for wheat grain and 0.05, 0.5, 3 mg/kg for straw. The supervised residue trials were carried out in 12 main wheat producing areas in China according to "guideline for the testing of pesticide residues in crops". The 35% suspension concentrate of bifenthrin and thiamethoxam was sprayed once at the dosage of 150 g/hm2 (active ingredient 52.5 g/hm2) at the beginning of wheat aphids bloom. The residual amounts of bifenthrin, thiamethoxam and clothianidin in wheat grains collected on day 14 and 21 after application verified the applicability of the MRL values, and the results of multi-point tests had higher reliability. The results of long-term and short-term dietary exposure risk assessment showed that the dietary exposure risks of bifenthrin, thiamethoxam and clothianidin residues in wheat were acceptable for children aged 1-6 years and the general population.
Determination and chronic dietary exposure assessment of procymidone residue in Chinese chives
Yong ZHOU, Xiuying PIAO, Xianjun LIAO, Jia LIU, Hang ZHU, Haihao MA, Xiaomao ZHOU, Fugen LI
2021, 23(2): 373-379.   doi: 10.16801/j.issn.1008-7303.2021.0007
[Abstract](251) [FullText HTML](179) [PDF 528KB](17)
Abstract:
An effective method was developed for the determination of procymidone residue in Chinese chives by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The supervised residue field trials of procymidone were designed and conducted in China (Heilongjiang, Liaoning, Henan, Shandong, Anhui, Hunan, Guangxi, and Fujian Province) in 2019. The risk of residue of procymidone applied in Chinese chives was studied, and the chronic dietary exposure risk of procymidone was evaluated. The samples were extracted by acetonitrile, purified with PSA and GCB, detected using HPLC-MS/MS, and quantified by external standard method. The recoveries ranged from 74% to 98% with the relative standard deviations (RSD) of 4.6%-9.9% at the fortified levels of 0.02 to 20 mg/kg. The limit of quantitation (LOQ) of the method was 0.02 mg/kg. The field trial results showed that after the spraying of 50% wettable powders (WP) of procymidone at 450 g a.i./ hm2 once, the final residues in Chinese chives from 8 provinces were 0.04-1.06 mg/kg at 30 days after the application. Given that the national estimated daily intake (NEDI) of procymidone was 2.5562 mg, its risk quotient (RQ) was 40.6%. The result of the chronic dietary exposure assessment revealed that it might not pose an unacceptable risk to the general population’s health by applying procymidone on Chinese chives.
Screening, residue dissipation and risk assessment of 54 pesticides in winter jujube under different harvesting and storage conditions
Jiangsheng MAO, Zilei CHEN, Changying GUO, Huidong LI, Ruiyan DING, Wenjun ZHANG, Mengmeng YAN
2021, 23(2): 380-387.   doi: 10.16801/j.issn.1008-7303.2021.0027
[Abstract](256) [FullText HTML](159) [PDF 622KB](14)
Abstract:
The effects of different storage time, storage temperature and harvesting period on pesticide residues in different circulation stages of winter jujube were studied by using GC-MS-MS and LC-MS-MS. And the risk assessment for the safe application of 12 kinds of pesticides in winter jujube was conducted. The results showed that, among the 54 pesticides tested, 12 of them were detected in the winter jujube samples, and the overall detection rate was 22.6%. No banned or highly toxic pesticides were detected. At room temperature, the half-life of carbendazim was 4.8-6.0 days, the half-life of pentazolidol was 4.9-11.2 days, and the half-life of phenyleocycloazole, imidacloprid, and pyrizoyl ester were 10.0 days, 2.8 days, and 6.9 days, respectively. Under the condition of 0 ℃, the half-life of carbendazim was 5.5-9.4 days, the half-life of pentazolidol was 14.1-57.8 days, and the half-life of phenyleocycloazole and imidacloprid were 8.6 days and 10.5 days, respectively. The dissipation of 9 pesticides in winter jujube at different harvesting stages was obvious. The dissipation of fresh jujube at commercial harvesting stage was higher than 50%. Studies on the risk assessment of chronic and acute dietary exposure to pesticide residues in winter jujube after different harvest and market procurements showed that the risk of dietary intake was low and acceptable, except for carbendazem. The chronic ingestion risks of carbendazim in winter jujube in different circulation periods (market procurement) were unacceptable.
Residue and dissipation of fluopicolide, its metabolite and propamocarb in the leaf lettuce using a modified QuEChERS method and HPLC-MS/MS
Hongxia TANG, Jiaqing HUANG, Qiang SUN, Guangyue WEN, Maofeng DONG, Weimin WANG
2021, 23(2): 388-394.   doi: 10.16801/j.issn.1008-7303.2021.0026
[Abstract](212) [FullText HTML](153) [PDF 868KB](13)
Abstract:
A modified QuEChERS approach had been developed for simultaneous determination of fluopicolide, its metabolite 2,6-dichlorobenzamide and propamocarb in the leaf lettuce by HPLC-MS/MS. The samples were extracted by acetonitrile with multi-wall carbon nanotubes (MWCNTs) for purification. The quantitative analysis of the samples achieved using the external standard of the matrix solution. The validation results showed that, in the range of 0.005-1 mg/L, the response of the concentrations of the compounds and the instruments had good linear relationship (R2 ≥ 0.999). Satisfied recoveries (85%-106%) and relative standard deviations (1.0%-18%) were obtained when spiked with 0.02, 0.1, 2, and 100 mg/kg in the samples. The acceptable limits of quantitation were 0.02 mg/kg for all the three compounds. In the field experiments, after sprayed by 928.13 g a.i./hm2 for 3 times and with a spraying interval of 7 d, the dissipation of fluopicolide and propamocarb in the leaf lettuce were following with the first-order kinetics equation, and their half-lives were 3.9-4.2 d for fluopicolide and 4.8-4.9 d for propamocarb, respectively. When the sample intervals were 5 d and 7 d, the residues levels of fluopicolide and propamocarb in the leaf lettuce were 3.45-8.51 mg/kg and 9.05-31.1 mg/kg, respectively. In terms of 2,6-dichlorobenzamide, the residues were lower than 0.02 mg/kg. Based on the growth characteristics and consumption habits of leaf lettuce, and the MRLs of China and Codex Alimentarius Commission (CAC), 5 d was selected as the post-harvest interval.
Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry
Qin YANG, Yaohai ZHANG, Jie ZHOU, Bining JIAO
2021, 23(2): 395-404.   doi: 10.16801/j.issn.1008-7303.2021.0056
[Abstract](203) [FullText HTML](127) [PDF 831KB](15)
Abstract:
In this study, a rapid multi-residue detection method for 75 pesticide residues in 5 citrus, including mandarin, orange, lemon, pummelo and kumquat, was developed. Pesticide residues were extracted from citrus by magnetic dispersive solid phase extraction (MDSPE)-QuEChERS pretreatment and analyzed by gas chromatography-tandem mass spectrometry(GC-MS/MS). Graphitized carbon black (GCB), primary secondary amine (PSA) and magnetic nanoparticles (MNPS) were used as adsorbents in the (MDSPE)-QuEChERS pretreatment. In order to obtain the optimum recovery rate of pesticide analysis, the amounts of the adsorbents were investigated. Under the optimized conditions, a simple, fast, safe, cheap, reproducible, and applicable multi-residue method was established. Acceptable linearity was maintained at the concentration of 0.01 to 0.5 mg/kg, the average recoveries were in the range of 63% to 118%, and the relative standard deviations (RSDs) ranged from 0.30% to 16%. Also, the limits of detection (LODs) ranged from 1 to 7 μg/kg and the limits of quantification (LOQs) were in the range of 10-20 μg/kg.
Determination of 126 pesticides residues in soybean oil by solid phase extraction-gas chromatography-tandem mass spectrometry
Chunming WANG, Yang ZHANG, Dongbin WANG, Pengfei SHI, Bo YANG
2021, 23(2): 405-413.   doi: 10.16801/j.issn.1008-7303.2021.0047
[Abstract](311) [FullText HTML](174) [PDF 1242KB](22)
Abstract:
A multi-residue analysis method was established for simultaneous determination of 126 pesticides in soybean oil using SPE-gas chromatography-tandem mass spectrometry (GC/MS/MS). The samples were degreased by n-hexane saturated with acetonitrile and extracted by n-hexane saturated acetonitrile under mechanical shaking. Then the extracts were centrifuged at −5 ℃ and 20000 r/min for 5 min, and cleaned-up with Captiva EMR-Lipid solid phase extraction column. After being re-dissolved with ethyl acetate, the samples were detected using multiple reaction monitoring (MRM) on GC-MS/MS system and quantified with external standard method using matrix matched calibration curves. The results showed that: in the range of 0.003-0.2 mg/L, good linear relationship were obtained between the concentrations of 126 pesticides and their corresponding peak areas, and the R2 was greater than 0.995. The recoveries of 126 pesticides ranged from 60% to 119% at the spiked levels of 0.005, 0.01 and 0.05 mg/kg. The RSDs were lower than 20% for 122 pesticides, and were lower than 25% for the other four pesticides. The method can effectively remove glycerolipid and some lipophilic interference from the soybean oil. The sensitivity, accuracy and precision of the method meet the requirements of pesticide residue detection. It provides an efficient and reliable analytical method for monitoring the level of pesticide residues in soybean oil and effectively preventing the health risks.
Detection of 4 pesticides residues in peanut using QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
Song YANG, Nan ZOU, Zheng YOU, Jie YU, Ling WANG, Li SU, Wei MU
2021, 23(2): 414-420.   doi: 10.16801/j.issn.1008-7303.2021.0023
[Abstract](781) [FullText HTML](356) [PDF 745KB](23)
Abstract:
A method was developed for simultaneous determination of the residues of quizalofop-p-ethyl, chlorpyrifos, acetochlor amd imidacloprid in peanut by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was purified with a combination of Nano-ZrO2, C18 and multi-walled carbon nanotubes (MWCNT), detected by UPLC-MS/MS, and quantified by external standard method. The results showed that in the range of 0.001-0.5 mg/L, the linear relationship between the mass concentrations of the 4 pesticides and their corresponding peak areas was good, with r≥0.9986. At the three spike levels of 0.01, 0.1 and 1 mg/kg, the average recoveries of the four pesticides in peanuts were between 82% and 109%. And the relative standard deviations (RSDs, n = 5) were between 2.8% and 9.0%. Among them, the limit of quantification (LOQ) was 0.01 mg/kg. This method was used to test 10 batches of peanut samples collected from large supermarkets and agricultural markets in Tai’an City. The results showed that the residues of the four pesticides in all samples did not exceed the maximum residue limits set by China. This method has the advantages of good purification effect, simple and efficient operation, high sensitivity, good stability and strong versatility. It is suitable for the simultaneous detection of four pesticide residues in peanuts.
Research Report
Design, synthesis and fungicidal activities of phenazine-1-carboxamida conjugates of 1,3,4-thia(oxa)diazole
Min HE, Jingwen GU, Sicheng LI, Xuwen XIANG, Shan JIANG, Zining CUI
2021, 23(2): 287-295.   doi: 10.16801/j.issn.1008-7303.2021.0022
[Abstract](245) [FullText HTML](191) [PDF 466KB](28)
Abstract:
Phenazine-1-carboxylic acid (PCA), isolated from Pseudomonas, is a very important fungicidal agent. PCA and its derivatives revealed good biological activities in the field of medicine and agrichemicals. In this paper, two series of PCA derivatives containing 1,3,4-thiadiazole and 1,3,4-oxadiazole were designed and synthesized to explore novel fungicidal candidates. Their in vitro and in vivo fungicidal activities were evaluated. The title compounds I 8 (X=S, R=2-OCH3) and I 22 (X=O, R=2-OCH3) had EC50 vaues of 33.25 μg/mL and 46.52 μg/mL against Fusarium graminearum, respectively, which were about 3-4 times better than of PCA (EC50 = 128.54 μg/mL). In vivo results showed that compounds I 8 and I 22 gave better bioactivity (inhibitory rates of 58.69% and 55.37% at 500 μg/mL, respectively) against F. graminearum than that of PCA (25.14%). Preliminary structure-activity relationship study found that the introduction of electron-donating groups were favored to improving the activity of the derivatives, and the substitution at ortho-position of benzene ring would be favored to fungicidal activity. The substitution position of the same substituent on the benzene ring was in the order of o > p > m according to the bioactivity.These results can be used to guide the further structural modification of these compounds for novel fungicidal agent.
Inhibitory activity of aloesin and aloe gel against Curvularia lunata
Guohui ZHANG, Rongyu LI, Xiaomao WU, Ming LI
2021, 23(2): 316-322.   doi: 10.16801/j.issn.1008-7303.2021.0018
[Abstract](363) [FullText HTML](211) [PDF 587KB](6)
Abstract:
In order to find natural active substance alternative to the chemical fungicides currently used against the devastating Curvularia leaf spot of rice, the bioactivity of aloesin and aloe gel against Curvularia lunata was determined. The filter paper method showed that 300 mg/mL aloesin led to an obvious inhibitory band (3.37 mm) at 28 h, and a inhibitory zone (Φ = 51.27 mm) against spores (3 × 104 cfu/mL), and these inhibitory effects remained until 6 d. The mycelial inhibition rate by aloe gel at 1, 2, 4, 8, 16, 32 and 64 mg/mL ranged from 9.25% to 56.21% at 5 d, and it increased with increased concentration. Additionally, the inhibition rate of 64 mg/mL aloe gel increased by 21.87% from 2 to 5 d. The mycelial growth of C. lunata treated with 160 mg/mL aloesin was weaker than control, and no appressorium produced. The germ tube of C. lunata treated with aloe gel was much slower than control, and the inhibition rate was 75.39%-96.58%. This study was first reported that aloesin effectively inhibited mycelia growth and conidia germination of C. lunata, and aloe gel effectively inhibited mycelia growth of C. lunata.
Research advances and application prospects of microencapsulation techniques in pesticide
LI Beixing, ZHANG Daxia, ZHANG Canguang, GUAN Lei, WANG Kai, LIU Feng
2014, 16(5): 483-496.   doi: 10.3969/j.issn.1008-7303.2014.05.01
[Abstract](4321) [PDF 1351KB](1005)
Research progresses on the metabolic mechanisms of organophosphate insecticides
Wang Zhichao, Kang Zhijiao, Shi Xueyan, Gao Xiwu
2015, 17(1): 1-14.   doi: 10.3969/j.issn.1008-7303.2015.01.01
[Abstract](4183) [PDF 1725KB](817)
Research progress and prospects of microbial pesticide formulation for plant disease control
LIU Zhenhua, LUO Yuanchan, ZHANG Daojing, LI Yuanguang
2014, 16(5): 497-507.   doi: 10.3969/j.issn.1008-7303.2014.05.02
[Abstract](4011) [PDF 1299KB](750)
Research progress on insecticides resistance in fall armyworm, Spodoptera frugiperda
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Preliminary studies on synergism and mechanisms of six organosilicon additives on fomesafen
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