王全胜, 张亮, 付岩, 凌淑萍, 吴银良. 噻二唑类农药在猕猴桃上的残留分析方法[J]. 农药学学报, 2022, 24(1): 197-202. DOI: 10.16801/j.issn.1008-7303.2021.0151
    引用本文: 王全胜, 张亮, 付岩, 凌淑萍, 吴银良. 噻二唑类农药在猕猴桃上的残留分析方法[J]. 农药学学报, 2022, 24(1): 197-202. DOI: 10.16801/j.issn.1008-7303.2021.0151
    WANG Quansheng, ZHANG Liang, FU Yan, LING Shuping, WU Yinliang. Residue analysis method of thiadiazole derived pesticides in kiwi fruit[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 197-202. DOI: 10.16801/j.issn.1008-7303.2021.0151
    Citation: WANG Quansheng, ZHANG Liang, FU Yan, LING Shuping, WU Yinliang. Residue analysis method of thiadiazole derived pesticides in kiwi fruit[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 197-202. DOI: 10.16801/j.issn.1008-7303.2021.0151

    噻二唑类农药在猕猴桃上的残留分析方法

    Residue analysis method of thiadiazole derived pesticides in kiwi fruit

    • 摘要: 为优化噻二唑类农药在猕猴桃中的残留分析方法,开发了基于改良QuEChERS法并结合超高效液相色谱-串联质谱(UPLC-MS/MS)的分析方法。目标物经氢氧化钠碱解、盐酸溶液调节pH值至2~3后转化为待测物噻二唑,再经乙腈提取、盐析分层、C18和石墨化碳黑吸附剂净化, UPLC-MS/MS检测。结果表明:在0.001 ~ 0.5 mg/L范围内,噻唑锌、噻菌铜、噻森铜和噻二唑基质标准工作液的质量浓度与响应值间均呈良好的线性关系,相关系数r≥0.999。在0.01 ~ 1 mg/kg添加水平下,噻唑锌、噻菌铜、噻森铜和噻二唑在猕猴桃中的平均回收率为81% ~ 93%,相对标准偏差 (RSD)最大为9.3%,表明方法的准确度和精密度均符合残留分析的要求。方法定量限 (LOQ)均为0.01 mg/kg,表明方法灵敏度较高。与现有传统分析方法相比,该方法普适性更大、灵敏度更高、更高效且前处理过程安全、环保,有助于提高噻二唑类农药的残留风险监测水平。

       

      Abstract: Aiming to optimize the residue analysis methods of thiadiazole derived pesticides in kiwi fruits, a method based on the modified QuEChERS method coupled with UPLC-MS/MS was developed. The target pesticides were transformed into thiadiazole by reacting with NaOH and adjusting the pH to 2 ~ 3 with HCl. Then thiadiazole was extracted with acetonitrile, salted out with NaCl, cleaned up with C18 and GCB, and detected with UPLC-MS/MS. The results showed that the correlation coefficient (r) was no less than 0.999 within the concentration range from 0.001 to 0.5 mg/L, which indicated a satisfactory linear relation between the areas and the concentrations of thiazole zinc(THIA), thiediazole copper(THIE), thiosen copper(THIO) and thiediazole(AMT). Meanwhile, the average recoveries of THIA, THIE, THIO and AMT were 81% ~ 93% with the maxium RSD of 9.3% at the spiked concentration of 0.01 to 1 mg/kg which indicated that the accuracy and precision of the method met the requirements of residue analysis. The limit of quantification (LOQ) was 0.01 mg/kg, showing the high sensitivity of the method. Compared with the exiting traditional methods, this new developed method has greater universality, higher sensitivity and more efficiency, and the sample preparation process is safer and environmental friendly, which is helpful to improve the residue risk monitoring levels of thiadiazole derived pesticides.

       

    /

    返回文章
    返回