| 液相色谱-串联质谱法测定月柿中187种农药残留 |
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| 基金项目:广西壮族自治区科技创新能力与条件建设计划（桂科能14123006-15，桂科能1598025-1） |
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| 中文摘要:建立了液相色谱-串联质谱检测广西月柿中187种农药残留的方法。试样采用含1%醋酸乙腈提取，经无水硫酸镁（MgSO4）、无水醋酸钠（CH3COONa）、无水硫酸钠（Na2SO4）、N 丙基乙二胺（PSA）和C18萃取净化。以含0005 mol/L甲酸铵和含001%甲酸的95%乙腈水溶液为有机相，含0005 mol/L甲酸铵和001%甲酸的水溶液为水相进行梯度洗脱。使用电喷雾离子源，正离子模式（ESI+）和动态多反应监测（DMRM）方式进行扫描检测，基质匹配外标法定量。187种农药在1~100 μg/kg范围内线性关系良好，相关系数（r2）大于099；方法检出限（S/N≥3）均为1 μg/kg，定量下限（S/N≥10）均为10 μg/kg；加标回收率为702%~118%，相对标准偏差为20%~20%（n=6）。该方法准确、灵敏、快速，适于月柿中农药多残留的高通量检测。 |
| 中文关键词:液相色谱-串联质谱 电喷雾正离子模式 月柿 农药多残留 |
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| Determination of 187 Pesticide Residues in Dried Persimmon by Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A method for the determination of 187 kinds of pesticides in dried persimmon by liquid chromatography-tandem mass spectrometry（LC-MS/MS） was established.The samples were extracted with acetonitrile containing 1% acetic acid，then purified with anhydrous magnesium sulfate，anhydrous sodium acetate，anhydrous sodium sulfate，N propyl ethylenediamine（PSA） and C18.The separation of targeted compounds was performed on a ZORBAX Eclipse Plus-C18 column by gradient elution using 95% acetonitrile aqueous solution（organic phase） and water（aqueous phase） as mobile phases，both contained 0005 mol/L ammonium formate and 001% formic acid.The compounds were detected by LC-MS/MS with positive electrospray ion source（ESI+） under dynamic multiple reaction monitoring（DMRM） mode.The matrix-matched external standard method was used for the quantitation.The callibration curves for 187 pesticides were linear in the range of 1-100 μg/kg with correlation coefficients（r2） more than 099.The limits of detection（S/N≥3） and quantitation（S/N≥10） for the analytes were 1 μg/kg and 10 μg/kg，respectively.The recoveries were in the range of 702%-118% with relative standard deviations（RSDs，n=6） of 20%-20%.The method is suitable for the high throughput detection on pesticide multi residues in dried persimmon with its advantages of accuracy，sensitivity and rapidness. |
| Key Words:liquid chromatography-tandem mass spectrometry（LC-MS/MS） positive electrospray ion source dried persimmon pesticide multi residue |
| 引用本文：秦富，邓全道，李湧，黄大新，汪文龙.液相色谱-串联质谱法测定月柿中187种农药残留[J].分析测试学报,2018,37(8):879-886. |
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