气相色谱-串联质谱动态多反应监测模式测定陈皮中88种农药残留

该文采用改进的QuEChERS结合气相色谱-串联质谱(GC-MS/MS)建立了陈皮中88种农药残留在动态多反应检测(dMRM)模式下的检测方法。对样品提取方式进行筛选优化,采用乙腈为提取剂,加入无水硫酸镁4.0 g、无水乙酸钠1.0 g、陶瓷均质子提取,以PSA 200 mg、C 18100 mg、GCB 30 mg净化,通过基质匹配外标法校正,减弱了陈皮中基质效应对目标化合物定量准确性的影响。结果表明,88种农药在一定浓度范围内的线性关系良好,相关系数(r 2)均不低于0.9963,以3倍信噪比(S/N=3)计算得方法检出限(LOD)为0.0010~0.0500 mg/kg,以S/N=10计算得定量下限(LOQ)为0.002~0.1000 mg/kg;在低、中、高3个加标浓度下的平均回收率为60.1%~118%,相对标准偏差(RSD)为0.30%~13%(n=6)。方法快速高效、灵敏可靠,适用于陈皮中农药残留的快速筛查及日常检测。

Determination of 88 Pesticide Residues in Pericarpium citri reticulatae by Gas Chromatography-Tandem Mass Spectrometry in Dynamic Multiple Reaction Monitoring Mode

An analytical method was established for the determination of 88 pesticide residues in Pericarpium citri reticulatae by improved QuEChERS pretreatment combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)in dynamic multi-reaction monitoring mode.Screening and optimizing of sample extraction methods,acetonitrile as extraction solvent,then added with 4.0 g anhydrous magnesium sulfate and 1.0 g anhydrous sodium acetate,followed by ceramic proton extraction,200 mg PSA,100 mg C 18 and 30 mg GCB purification,and finally corrected by matrix matching external standard method.Influences of matrix effect on the quantification accuracy for target compounds in Pericarpium citri reticulatae were significantly weakened.The calibration curves for 88 pesticides exhibited good linearity in a certain concentration range,with their correlation coefficients(r 2)not less than 0.9963.The limits of detection(S/N=3)and the limits of quantification(S/N=10)were 0.0010-0.0500 mg/kg and 0.002-0.1000 mg/kg,respectively.Moreover,the average recoveries at low,medium and high spiked levels ranged from 60.1%to 118%with the relative standard deviations(RSDs,n=6)ranged from 0.30%to 13%.The method was fast,efficient,sensitive and reliable,and was suitable for the rapid screening and routine detection of pesticide residues in Pericarpium citri reticulatae.