气相色谱-三重四极杆串联质谱法测定食药同源物质中10种农药残留

Determination of 10 Pesticide Residues in Food and Drug Homologous Substances by Gas Chromatography Triple Quadrupole Tandem Mass Spectrometry

目的:建立基于保留指数原理气相色谱-三重四极杆串联质谱法测定铁皮石斛、灵芝、黄芪等药食同源物质中10种农药残留的方法。方法:采用Qu ECh ERS前处理方法进行样品中农药残留的提取、净化,结合气相色谱保留时间锁定技术,采用气质联用法测定,多反应监测模式,内标法定量。结果:在0.025~1.000 mg·L^(-1),10种农药线性关系良好,相关系数均大于0.997;在50μg·L^(-1)、100μg·L^(-1)、500μg·L^(-1)添加水平下,加标回收率在87.5%~109.3%,相对标准偏差在0.62%~6.35%;方法的检出限为0.001~0.002 mg·kg^(-1),定量限为0.0025~0.0060 mg·kg^(-1)。结论:该方法快速、方便,定性定量准确,结果可靠,适用于药食同源物质中多组分农药残留的测定。

Objective:To establish a gas chromatography-triple quadrupole tandem mass spectrometry method based on the retention index principle for the determination of 10 pesticide residues in food and drug homologous substances such as Dendrobium officinale,Ganoderma lucidum,Astragalus membranaceus.Method:The QuEChERS pre-treatment method is used for the extraction and purification of pesticide residues in samples,combined with gas chromatography retention time locking technology.gas chromatography-mass spectrometry is used for determination,multi reaction monitoring mode,and internal standard method is used for quantification.Result:The linear relationship between the 10 pesticides was good at 0.025~1.000 mg·L^(-1),and the correlation coefficients were all greater than 0.997;at the addition level of 50μg·L^(-1),100μg·L^(-1),500μg·L^(-1),the recovery rate of the added standard is between 87.5%and 109.3%,and the relative standard deviation is between 0.62%and 6.35%;the detection limit of the method is 0.001~0.002 mg·kg^(-1),and the quantitative limit is 0.0025~0.0060 mg·kg^(-1).Conclusion:This method is fast,convenient,accurate in qualitative and quantitative analysis,reliable in results,and suitable for the determination of multi-component pesticide residues in medicinal and food homologous substances.