气相色谱-串联质谱法测定花椒中106种农药残留及膳食暴露风险评估  

Determination of 106 pesticide residues by gas chromatography-tandem mass spectrometry and dietary exposure risk assessment in Chinese prickly ash

作　　者：陈敏[1] 尹全[1] 邓强[1] 刘茜 张义蓉[1] 杨晓凤[1] CHEN Min;YIN Quan;DENG Qiang;LIU Qian;ZHANG Yirong;YANG Xiaofeng(Institute of Quality and Testing Technology for Agro-products of Sichuan Academy of Agricultural Sciences,Chengdu 610066,China)

机构地区：[1]四川省农业科学院农业质量标准与检测技术研究所,成都610066

出　　处：《分析试验室》2024年第1期70-78,共9页Chinese Journal of Analysis Laboratory

基　　金：四川省农业科学院院列项目(2022ZZCX040)资助。

摘　　要：建立了固相萃取结合气相色谱-串联质谱(GC-MS/MS)测定花椒中106种农药残留量的方法。采用多反应监测(MRM)模式检测,基质匹配标准曲线法定量。结果表明:106种农药的定量限(LOQ)范围为0.010~0.10 mg/kg,且在定量限~1.0 mg/L范围内线性关系良好,线性相关系数R2≥0.99。106种农药的平均加标回收率在60.8%~118.6%之间,相对标准偏差(RSD)在0.79%~19%之间。将该方法用于53批次市售花椒样品的筛查,结果检出21种农药残留,其中有最大残留限量值(MRL)的农药有9种,无MRL值的农药有12种。无MRL值的农药慢性膳食摄入风险值(ADI)为0.002%~0.343%,12种农药ADI总计为1.03%,花椒中农药残留的膳食摄入风险较低。A method for the determination of 106 pesticide residues in Chinese prickly ash by solid phase extraction(SPE) combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed.The samples were detected by multiple-reaction monitoring scanning and quantified using the matrix-matched standard calibration method.The results showed that the limits of quantification(LOQs) of 106 pesticides ranged from 0.010 to 0.10 mg/kg.There were good linear relationships in the range of LODs-1.0 mg/L,with the correlation coefficients R2≥0.99.The average recoveries for the 106 pesticides at three spiked levels were 60.8%-118.6%,and the relative standard deviations(RSDs) were between 0.79% and 19%.The method was applied to the screening of 53 sample batches,the results showed that 21 pesticide residues were detected,including 9kinds with maximum residue limits(MRLs) for pesticides and 12 kinds without MRLs.The chronic dietary intake risk(ADI) was 0.002%-0.343%,and the total ADI of 12 pesticides was 1.03%,so the dietary intake risk of pesticide residues in Chinese prickly ash was low.

关 键 词：气相色谱-串联质谱 花椒 固相萃取 农药多残留 膳食风险评估 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]