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(Mg SO_4)、无水醋酸钠(CH_3COONa)、无水硫酸钠(Na_2SO_4)、N-丙基乙二胺(PSA)和C_(18)萃取净化。以含0.005 mol/L甲酸铵和含0.01%甲酸的95%乙腈水溶液为有机相,含0.005 mol/L甲酸铵和0.01%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(DM-RM)方式进行扫描检测,基质匹配外标法定量。187种农药在1~100μg/kg范围内线性关系良好,相关系数(r^2)大于0.99;方法检出限(S/N≥3)均为1μg/kg,定量下限(S/N≥10)均为10μg/kg;加标回收率为70.2%~118%,相对标准偏差为2.0%~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。
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 C 18.The separation of targeted compounds was performed on a ZORBAX Eclipse Plus-C 18 column by gradient elution using 95%acetonitrile aqueous solution(organic phase)and water(aqueous phase)as mobile phases,both contained 0.005 mol/L ammonium formate and 0.01%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 1-100μg/kg with correlation coefficients(r 2)more than 0.99.The limits of detection(S/N≥3)and quantitation(S/N≥10)for the analytes were 1μg/kg and 10μg/kg,respectively.The recoveries were in the range of 70.2%-118%with relative standard deviations(RSDs,n=6)of 2.0%-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.
作者
秦富
邓全道
李湧
黄大新
汪文龙
QIN Fu;DENG Quan-dao;LI Yong;HUANG Da-xin;WANG Wen-long(Inspection and Quarantine Technology Center of Guangxi Entry-Exit Inspection and Quarantine Bureau,Nanning 530021,China;Guilin Entry-Exit Inspection and Quarantine Bureau,Guilin 541004,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第8期879-886,共8页
Journal of Instrumental Analysis
基金
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)
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
liquid chromatography-tandem mass spectrometry(LC-MS/MS)
positive electrospray ion source
dried persimmon
pesticide multi-residue
