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磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留

杨秦 张耀海 周杰 焦必宁

杨秦, 张耀海, 周杰, 焦必宁. 磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留[J]. 农药学学报, 2021, 23(2): 395-404. doi: 10.16801/j.issn.1008-7303.2021.0056
引用本文: 杨秦, 张耀海, 周杰, 焦必宁. 磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留[J]. 农药学学报, 2021, 23(2): 395-404. doi: 10.16801/j.issn.1008-7303.2021.0056
Qin YANG, Yaohai ZHANG, Jie ZHOU, Bining JIAO. Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 395-404. doi: 10.16801/j.issn.1008-7303.2021.0056
Citation: Qin YANG, Yaohai ZHANG, Jie ZHOU, Bining JIAO. Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 395-404. doi: 10.16801/j.issn.1008-7303.2021.0056

磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留

doi: 10.16801/j.issn.1008-7303.2021.0056
基金项目: 国家重点研发计划 (2019YFC1605604);现代农业 (柑橘) 产业技术体系 (CARS-26):国家农产品质量安全风险评估重大专项 (GJFP2019012)
详细信息
    作者简介:

    杨秦,女,硕士研究生,E-mail:yangqin252423@163.com

    通讯作者:

    焦必宁,通信作者 (Author for correspondence),男,研究员,研究方向为果蔬质量安全及检测技术,E-mail:jiaobining@cric.cn

  • 中图分类号: S482;O657.7

Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry

  • 摘要: 基于磁性分散固相萃取 (MDSPE)-QuEChERS前处理技术,采用气相色谱-串联质谱法 (GC-MS/MS) 进行定性定量分析,建立了快速检测宽皮柑橘、甜橙、柠檬、柚子和金桔5种柑橘基质中75种农药残留的方法,优化了石墨化碳黑 (GCB)、N-丙基乙二胺 (PSA) 和磁性纳米粒子 (MNPS) 用量对不同柑橘中目标分析物回收率的影响。在优化条件下,目标分析物的线性范围在0.01~0.5 mg/kg之间,平均回收率为63%~118%,相对标准偏差为0.30%~16%。方法的检出限 (LOD) 为1~7 μg/kg,定量限 (LOQ) 为10~20 μg/kg。该方法简便、快速、安全、价格低廉,重现性良好,可用于不同柑橘中多种农药残留的快速确证检测。
  • 图  1  75种农药总离子流图 (Q3 Scan)

    Figure  1.  Total ion current diagram of 75 pesticides (Q3 Scan)

    图  2  GCB用量对农药回收率的影响

    1. 敌敌畏dichlorvos; 2. 2,4,6,-三氯苯酚 2,4,6-TCP; 3.嘧霉胺pyrimethanil; 4. 百菌清chlorothalonil; 5. 毒死蜱chlorpyrifos; 6. 三唑酮triadimefon; 7. 杀扑磷methidathion; 8. 丙溴磷profenofos; 9. 烯唑醇diniconazole; 10. 三唑磷triazophos; 11. 联苯菊酯bifenthrin; 12. 甲氰菊酯fenpropathrin; 13. 高效氯氟氰菊酯lambda-cyhalothrin; 14. 氰戊菊酯-1 fenvalerate-1; 15. 氰戊菊酯-2 fenvalerate-2.

    Figure  2.  The effect of different dosages of GCB on the pesticide recoveries

    图  3  PSA用量对农药回收率的影响

    1. 敌敌畏dichlorvos; 2. 2,4,6,-三氯苯酚 2,4,6-TCP; 3. 嘧霉胺pyrimethanil; 4. 百菌清chlorothalonil; 5. 毒死蜱chlorpyrifos; 6. 三唑酮triadimefon; 7. 杀扑磷methidathion; 8. 丙溴磷profenofos; 9. 烯唑醇diniconazole; 10. 三唑磷triazophos; 11. 联苯菊酯bifenthrin; 12. 甲氰菊酯fenpropathrin; 13. 高效氯氟氰菊酯lambda-cyhalothrin; 14. 氰戊菊酯-1 fenvalerate-1; 15. 氰戊菊酯-2 fenvalerate-2.

    Figure  3.  The effect of different dosages' of PSA on the pesticide recoveries

    图  4  MNPS用量对农药回收率的影响

    1. 敌敌畏dichlorvos; 2. 2,4,6,-三氯苯酚 2,4,6-TCP; 3. 嘧霉胺pyrimethanil; 4. 百菌清chlorothalonil; 5. 毒死蜱chlorpyrifos; 6. 三唑酮triadimefon; 7. 杀扑磷methidathion; 8. 丙溴磷profenofos; 9. 烯唑醇diniconazole; 10. 三唑磷triazophos; 11. 联苯菊酯bifenthrin; 12. 甲氰菊酯fenpropathrin; 13. 高效氯氟氰菊酯lambda-cyhalothrin; 14. 氰戊菊酯-1 fenvalerate-1; 15. 氰戊菊酯-2 fenvalerate-2.

    Figure  4.  The effect of different dosages of MNPS on the recoveries

    图  5  添加MNPS前 (A) 后 (B) 温州蜜柑净化对比图

    Figure  5.  Chromatograms of mandarin extract after clean-up procedure before (A) or after (B) MNPS spiked

    表  1  75种农药标准品纯度、保留时间及GC-MS/MS的质谱条件

    Table  1.   Retention time of 75 pesticides and mass spectrometry conditions of GC-MS/MS

    序号
    No.
    农药      
    Pesticide      
    纯度/浓度
    Purity/concentration
    保留时间
    Retention time/min
    定量离子
    Quantitative ion, m/z
    定性离子
    Qualitative ion, m/z
    碰撞能量
    CE/eV
    1 敌敌畏 dichlorvos3) > 99% 4.585 109.0 > 79.0 185.0 > 93.0 8, 14
    2 2,4,6,-三氯苯酚 2,4,6-TCP3) > 99.2% 5.170 132.0 > 97.0 196.0 > 132.0 10, 15
    3 邻苯基苯酚 2-phenylphenol3) > 98% 6.085 170.1 > 141.1 141.1 > 115.1 24, 18
    4 灭线磷 ethoprophos3) > 97.5% 6.775 200.0 > 158.0 158.0 > 97.0 6, 18
    5 久效磷 monocrotophos3) > 98% 7.005 127.1 > 109.0 127.1 > 95.0 12, 16
    6 治螟磷 sulfotep1) 1000 mg/L 7.010 322.0 > 202.0 322.0 > 174.0 10, 18
    7 硫线磷 cadusafos1) 1000 mg/L 7.155 158.9 > 130.9 158.9 > 97.0 8, 18
    8 甲拌磷 phorate3) > 96% 7.235 260.0 > 75.0 231.0 > 129.0 8, 24
    9 α-六六六 α-HCH3) > 97.5% 7.395 180.9 > 144.9 218.9 > 182.9 16, 8
    10 乐果 dimethoate3) > 99.5% 7.505 125.0 > 47.0 125.0 > 79.0 14, 8
    11 β-六六六 β-HCH3) > 97.5% 7.735 180.9 > 144.9 218.9 > 182.9 16, 8
    12 特丁硫磷 terbufos1) 1000 mg/L 7.900 231.0 > 128.9 231.0 > 174.9 26, 14
    13 γ-六六六 γ-HCH3) > 99% 7.925 180.9 > 144.9 218.9 > 182.9 16, 8
    14 嘧霉胺 pyrimethanil3) > 98.3% 8.085 198.1 > 183.1 198.1 > 118.1 14, 28
    15 氯唑磷 isazofos3) > 95% 8.160 257.0 > 162.0 257.0 > 119.0 8, 18
    16 百菌清 chlorothalonil3) > 99.3% 8.170 263.9 > 168.0 263.9 > 228.8 24, 18
    17 δ-六六六 δ-HCH3) > 99.1% 8.330 180.9 > 144.9 218.9 > 182.9 16, 8
    18 抗蚜威 pirimicarb3) > 99.3% 8.375 238.1 > 166.1 166.1 > 55.0 12, 20
    19 甲基对硫磷 parathion-methyl3) > 98.5% 8.955 263.0 > 109.0 125.0 > 47.0 14, 12
    20 精甲霜灵 metalaxyl-M 3) > 98% 9.080 249.0 > 146.0 249.0 > 160.0 15, 13
    21 七氯 heptachlor3) > 99% 9.215 271.8 > 236.9 273.8 > 238.9 20, 16
    22 杀螟硫磷 fenitrothion3) > 98% 9.405 277.0 > 260.0 277.0 > 109.1 6, 14
    23 马拉硫磷 malathion1) 1000 mg/L 9.530 173.1 > 99.0 173.1 > 127.0 14, 6
    24 毒死蜱 chlorpyrifos3) > 99.9% 9.715 196.9 > 168.9 313.9 > 257.9 14, 14
    25 倍硫磷 fenthion3) > 99% 9.790 278.0 > 109.0 278.0 > 169.0 20, 14
    26 对硫磷 parathion3) > 98.7% 9.865 139.0 > 109.0 291.1 > 109.0 8, 14
    27 艾氏剂 aldrin3) > 97% 9.915 262.9 > 191.0 262.9 > 193.0 34, 28
    28 三唑酮 triadimefon3) > 99.7% 9.920 208.1 > 181.0 208.1 > 111.0 10, 22
    29 水胺硫磷 isocarbophos1) 1000 mg/L 9.940 289.1 > 136.0 230.0 > 212.0 14, 10
    30 三氯杀螨醇 dicofol1) 1000 mg/L 10.050 139.0 > 111.0 139.0 > 75.0 16, 28
    31 甲基异柳磷 isofenphos-methyl1) 1000 mg/L 10.245 199.0 > 121.0 241.1 > 121.1 14, 22
    32 氟虫腈 fipronil1) 1000 mg/L 10.410 366.9 > 212.9 368.9 > 214.9 30, 30
    33 硫环磷 phosfolan3) > 99% 10.580 255.0 > 227.0 255.0 > 140.0 6, 22
    34 环氧七氯 (exo) heptachlor exo-epoxide2) 100 mg/L 10.655 352.8 > 262.9 354.8 > 264.9 14, 20
    36 喹硫磷 quinalphos1) 1000 mg/L 10.710 146.1 > 118.0 146.1 > 91.0 10, 24
    37 环氧七氯 (endo) heptachlor-epoxide2) 100 mg/L 10.730 352.8 > 253.0 354.8 > 253.0 26, 18
    38 杀扑磷 methidathion3) > 99.5% 11.015 145.0 > 85.0 145.0 > 58.0 8, 14
    39 氯丹-反式 trans-chlordane1) 1000 mg/L 11.095 373.0 > 337.0 272.0 > 237.0 10, 15
    40 氯丹-顺式 cis-chlordane1) 1000 mg/L 11.130 375.0 > 303.0 375.0 > 266.0 10, 20
    41 苯硫威 fenothiocarb3) > 96.5% 11.200 160.1 > 72.0 160.1 > 106.1 10, 12
    42 苯线磷 fenamiphos3) > 93% 11.395 303.1 > 195.1 288.1 > 260.1 8, 6
    43 咯菌腈 fludioxonil3) > 99% 11.545 248.0 > 127.0 248.0 > 154.0 26, 20
    44 丙溴磷 profenofos3) > 98.5% 11.690 338.9 > 268.9 336.9 > 266.9 18, 14
    45 4,4′-滴滴伊 p,p′-DDE3) > 99% 11.805 246.0 > 176.0 317.9 > 248.0 30, 24
    46 腈菌唑 myclobutanil3) > 99% 11.840 179.1 > 125.0 179.1 > 152.0 14, 8
    47 氟硅唑 flusilazole3) > 98% 11.895 233.1 > 165.1 206.1 > 151.1 14, 16
    48 狄氏剂 dieldrin3) > 99.2% 11.980 276.9 > 241.0 262.9 > 193.0 8, 34
    49 异狄氏剂 endrin1) 1000 mg/L 12.430 262.9 > 191.0 262.9 > 193.0 30, 28
    50 烯唑醇 diniconazole3) > 99% 12.595 268.0 > 232.0 270.0 > 234.0 12, 10
    51 4,4′-滴滴滴 p,p′-DDD1) 1000 mg/L 12.760 235.0 > 165.0 237.0 > 165.0 24, 28
    52 2,4′-滴滴涕 o,p′-DDT1) 1000 mg/L 12.775 235.0 > 165.0 237.0 > 165.0 24, 28
    53 三唑磷 triazophos3) > 97% 12.950 161.0 > 134.0 161.0 > 106.0 8, 14
    54 异狄氏剂醛 endrin-aldehyde1) 100 mg/L 12.950 345.0 > 245.0 345.0 > 281.0 15, 30
    55 肟菌酯 trifloxystrobin3) > 99% 13.220 222.1 > 190.1 222.1 > 130.1 4, 12
    56 4,4′-滴滴涕 p,p′-DDT1) 1000 mg/L 13.515 235.0 > 165.0 237.0 > 165.0 24, 28
    57 戊唑醇 tebuconazole3) > 98.5% 13.800 250.1 > 125.1 125.1 > 89.0 22, 18
    58 炔螨特-1 propargite-13) > 95% 13.810 135.1 > 107.1 135.1 > 77.0 16, 24
    59 炔螨特-2 propargite-23) > 95% 13.835 135.1 > 107.1 135.1 > 77.0 16, 24
    60 异狄氏剂酮 endrin-ketone1) 100 mg/L 14.480 316.9 > 244.9 314.9 > 242.9 20, 18
    61 亚胺硫磷 phosmet3) > 98.5% 14.500 160.0 > 77.0 160.0 > 133.0 24, 14
    62 联苯菊酯 bifenthrin3) > 97.7% 14.505 181.1 > 166.1 181.1 > 179.1 12, 12
    63 溴螨酯 bromopropylate3) > 98% 14.605 340.9 > 182.9 340.9 > 184.9 18, 20
    64 联苯肼酯 bifenazate3) > 98% 14.630 300.1 > 258.1 258.1 > 196.1 8, 12
    65 甲氰菊酯 fenpropathrin3) > 98.5% 14.735 181.1 > 152.1 265.1 > 210.1 22, 12
    66 甲基谷硫磷 azinphos-methyl1) 100 mg/L 15.395 160.1 > 132.1 160.1 > 77.0 6, 20
    67 高效氯氟氰菊酯 lambda-cyhalothrin1) 1000 mg/L 15.685 181.1 > 152.1 163.1 > 91.0 24, 22
    68 灭蚁灵 mirex3) > 98% 15.900 271.8 > 236.8 273.8 > 238.8 18, 18
    69 螺螨酯 spirodiclofen3) > 98% 16.545 312.0 > 109.0 312.0 > 259.0 20, 12
    70 蝇毒磷 coumaphos3) > 98% 16.830 362.0 > 109.0 362.0 > 226.0 16, 14
    71 哒螨灵 pyridaben3) > 99% 16.885 147.1 > 117.1 147.1 > 132.1 22, 14
    72 氟氯氰菊酯-1 cyfluthrin-13) > 98.7% 17.410 163.1 > 127.1 163.1 > 91.0 6, 14
    73 氟氯氰菊酯-2 cyfluthrin-23) > 98.7% 17.525 163.1 > 127.1 163.1 > 91.0 6, 14
    74 氟氯氰菊酯-3 cyfluthrin-33) > 98.7% 17.615 163.1 > 127.1 163.1 > 91.0 6, 14
    75 氟氯氰菊酯-4 cyfluthrin-43) > 98.7% 17.680 163.1 > 127.1 163.1 > 91.0 6, 14
    76 氯氰菊酯-1 cypermethrin-11) 1000 mg/L 17.870 163.1 > 127.1 163.1 > 91.0 6, 14
    77 啶酰菌胺 boscalid3) > 99.5% 17.975 140.1 > 112.1 140.1 > 76.0 12, 24
    78 氯氰菊酯-2 cypermethrin-21) 1000 mg/L 18.030 163.1 > 127.1 163.1 > 91.0 6, 14
    79 氯氰菊酯-3 cypermethrin-31) 1000 mg/L 18.120 163.1 > 127.1 163.1 > 91.0 6, 14
    80 氯氰菊酯-4 cypermethrin-41) 1000 mg/L 18.190 163.1 > 127.1 163.1 > 91.0 6, 14
    81 氰戊菊酯-1 fenvalerate-13) > 97.7% 19.435 225.1 > 119.1 225.1 > 147.1 20, 10
    82 氰戊菊酯-2 fenvalerate-23) > 97.7% 19.850 225.1 > 119.1 225.1 > 147.1 20, 10
    83 溴氰菊酯-1 δmethrin-13) > 98% 20.610 180.9 > 151.9 252.9 > 93.0 22, 20
    84 溴氰菊酯-2 δmethrin-23) > 98% 21.070 180.9 > 151.9 252.9 > 93.0 22, 20
    85 嘧菌酯 azoxystrobin3) > 99.2% 21.455 344.1 > 329.1 388.1 > 345.1 16, 18
    注:1)购自农业农村部环境保护科研监测所;2)购自上海农药;3)购自德国Dr. Ehrenstorfer。Note: 1)Purchased from the Environmental Protection Research and Monitoring Institute of the Ministry of Agriculture and Rural Affairs; 2)Purchased from Shanghai Pesticide; 3)Purchased from Dr. Ehrenstorfer, Germany.
    下载: 导出CSV

    表  2  五种柑橘基质的基质效应、检出限和定量限

    Table  2.   Matrix effects, LOD and LOQ of the five citrus matrices

    农药   
    Pesticide   
    基质效应
    Matrix effects
    检出限
    LOD/(μg/kg)
    定量限
    LOQ/(μg/kg)
    宽皮柑橘
    Mandarin
    甜橙
    Orange
    柠檬
    Lemon
    柚子
    Pummelo
    金桔
    Kumquat
    敌敌畏 dichlorvos 2.18 4.31 24.54 3.11 1.71 3~4 10~20
    2,4,6,-三氯苯酚 2,4,6-TCP 1.79 1.75 1.89 1.64 1.71 1 10
    邻苯基苯酚 2-phenylphenol 2.49 2.40 2.70 2.12 2.23 1 10
    灭线磷 ethoprophos 2.85 2.98 2.89 2.81 3.01 1 10
    久效磷 monocrotophos 14.90 20.13 20.16 22.70 28.55 3~6 10~20
    治螟磷 sulfotep 2.45 2.55 2.46 2.41 2.52 1 10
    硫线磷 cadusafos 8.41 8.69 8.70 8.18 8.48 4~6 20
    甲拌磷 phorate 2.35 2.43 2.14 2.31 2.39 1 10
    α-六六六 α-HCH 2.11 2.15 2.13 2.00 2.08 1 10
    乐果 dimethoate 12.09 13.74 16.26 14.13 15.84 1 10
    特丁硫磷 terbufos 3.02 3.18 2.64 3.00 3.09 1 10
    γ-六六六 γ-HCH 2.16 2.22 2.10 2.13 2.19 1~2 10
    嘧霉胺 pyrimethanil 5.78 5.99 8.04 4.93 4.44 1 10
    氯唑磷 isazofos 3.79 3.93 3.74 3.71 3.83 1 10
    百菌清 chlorothalonil 3.17 3.20 3.63 2.95 1.43 1 10
    δ-六六六 δ-HCH 9.91 9.99 9.86 9.71 9.86 1 10
    抗蚜威 pirimicarb 2.21 2.33 0.01 2.24 2.27 1~2 10
    甲基对硫磷 parathion-methyl 4.27 4.68 6.03 4.61 4.63 1 10
    精甲霜灵 metalaxyl-M 2.00 2.07 2.05 2.01 2.06 1 10
    七氯 heptachlor 1.99 2.06 2.06 1.99 2.02 1 10
    杀螟硫磷 fenitrothion 3.56 3.86 4.54 3.81 3.79 1 10
    马拉硫磷 malathion 2.79 3.29 3.41 3.27 3.30 1 10
    毒死蜱 chlorpyrifos 2.26 2.36 2.30 2.28 2.32 1 10
    倍硫磷 fenthion 2.78 2.89 2.80 2.78 2.83 1 10
    对硫磷 parathion 4.56 4.48 3.82 3.94 4.11 1~4 10
    艾氏剂 aldrin 1.52 1.51 1.43 1.44 1.51 1 10
    三唑酮 triadimefon 2.76 2.84 2.82 2.72 2.79 1 10
    水胺硫磷 isocarbophos 4.29 4.49 3.10 4.34 4.43 1 10
    三氯杀螨醇 dicofol 0.96 1.10 0.74 1.18 1.60 1 10
    甲基异柳磷 isofenphos-methyl 2.72 2.81 2.66 2.70 2.75 1 10
    氟虫腈 fipronil 3.34 3.50 3.45 3.32 3.39 1 10
    硫环磷 phosfolan 2.67 2.87 0.17 3.08 2.44 2~6 10~20
    环氧七氯 heptachlor 1.46 1.50 1.43 1.45 1.48 1 10
    稻丰散 phenthoate 2.87 2.97 2.87 2.89 2.98 1 10
    喹硫磷 quinalphos 2.50 2.61 1.93 2.58 2.59 1~2 10
    杀扑磷 methidathion 2.43 2.78 1.76 2.89 3.18 1 10
    氯丹 chlordane 1.46 1.53 1.44 1.59 1.65 1 10
    苯硫威 fenothiocarb 1.50 1.57 1.77 1.41 1.68 1 10
    苯线磷 fenamiphos 2.47 2.67 2.30 2.67 2.66 1 10
    咯菌腈 fludioxonil 1.46 1.47 1.52 1.49 1.27 1 10
    丙溴磷 profenofos 2.52 2.63 2.56 2.63 2.70 1 10
    4,4'-滴滴伊 p,p'-DDE 1.50 1.51 1.43 1.45 1.49 1 10
    腈菌唑 myclobutanil 2.57 2.62 2.38 2.65 2.58 1 10
    氟硅唑 flusilazole 2.49 2.51 2.27 2.52 2.51 1 10
    狄氏剂 dieldrin 1.40 1.43 1.35 1.36 1.42 1 10
    异狄氏剂 endrin 1.77 1.81 0.97 1.77 1.81 1~2 10
    烯唑醇 diniconazole 2.93 3.05 2.70 2.94 2.98 1 10
    4,4'-滴滴滴 p,p'-DDD 1.60 3.54 1.80 1.33 1.96 1 10
    2,4'-滴滴涕 o,p'-DDT 2.46 2.43 2.22 2.44 2.48 1 10
    三唑磷 triazophos 3.17 3.39 2.62 3.60 3.59 2~3 10
    异狄氏剂醛 endrin-aldehyde 1.02 0.11 1.13 0.97 1.09 1~2 10
    肟菌酯 trifloxystrobin 2.51 2.69 2.35 2.58 2.58 1 10
    4,4'-滴滴涕 p,p'-DDT 3.01 3.15 3.15 3.10 3.03 1 10
    戊唑醇 tebuconazole 3.06 3.26 3.12 3.30 3.20 1 10
    炔螨特 propargite 2.04 2.19 1.88 2.01 2.21 3~5 10~20
    异狄氏剂酮 endrin-ketone 1.59 1.64 1.94 1.60 1.61 1 10
    亚胺硫磷 phosmet 1.23 1.65 2.64 2.15 2.19 1~3 10
    联苯菊酯 bifenthrin 1.87 1.91 1.82 1.86 1.90 1 10
    溴螨酯 bromopropylate 2.26 2.31 2.23 2.28 2.31 1 10
    联苯肼酯 bifenazate 2.76 1.85 0.11 1.25 2.71 1~2 10
    甲氰菊酯 fenpropathrin 1.82 1.89 1.80 1.84 1.96 1~2 10
    甲基谷硫磷 azinphos-methyl 0.68 1.14 0.04 2.03 1.62 1~6 10~20
    高效氯氟氰菊酯 lambda-cyhalothrin 1.55 1.53 1.83 2.04 1.52 1~3 10
    灭蚁灵 mirex 1.29 1.32 1.27 1.27 1.28 1 10
    螺螨酯 spirodiclofen 10.37 10.67 7.75 10.86 10.90 1 10
    蝇毒磷 coumaphos 1.80 2.08 2.20 2.27 2.00 1 10
    哒螨灵 pyridaben 1.46 1.53 1.83 1.52 1.50 1 10
    氟氯氰菊酯 cyfluthrin 2.17 2.30 2.14 2.19 1.95 1~2 10
    氯氰菊酯 cypermethrin 1.57 2.07 1.89 1.68 1.84 1~3 10
    啶酰菌胺 boscalid 2.05 1.65 0.97 2.02 1.62 1~4 10
    氰戊菊酯 fenvalerate 2.44 2.53 2.31 2.41 2.26 1 10
    溴氰菊酯 deltamethrin 3.15 3.37 3.38 3.15 2.76 2~3 10
    嘧菌酯 azoxystrobin 5.26 5.39 2.74 4.90 4.24 1 10
    注:检出限和定量限是该农药在5种柑橘基质中的范围。Note: the LODs and the LOQs are the ranges of the pesticide in 5 citrus matrices.
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