茶叶中653种农药化学品残留GC-MS、GC-MS/MS与LC-MS/MS分析方法：国际AOAC方法评价预研究

Determination of 653 Pesticides and Chemical Contaminants Residues in Tea by GC-MS,GC-MS/MS and LC-MS/MS:the Pre-collaborative Study of AOAC Method Efficiency Evaluation

选择了16个实验室,按AOAC方法评价指南对盲样进行了检测。对16个实验室的统计分析结果表明:剔除操作偏离方法的2个实验室的全部数据,剩余14个实验室GC-MS/SIM(GC-MS/MS):RSDr<8%的占100%;RSDR<16%的占57.5%,RSDR<25%的占92.5%;HorRat值小于1.0的占80.0%,HorRat值小于2.0的占97.5%。LC-MS/MS:RSDr<8%的占65.0%,RSDr<15%的占97.5%;RSDR<16%的占35.0%,RSDR<25%的占95.0%;HorRat值小于1.0的占92.5%,HorRat值小于2.0的占97.5%。建立的1 220条标准曲线中,有1 132个满足r2≥0.995的要求,占92.8%;检测目标农药离子3 600个,离子丰度符合EU要求的有3 443个,占95.6%。AOAC方法评价结果证明,该方法重现性和再现性良好,完全适用于茶叶中653农药残留的定性和定量分析。

In this paper,16 laboratories were chosen through open recruitment on the internet and verifications of their qualifications,and international AOAC collaborative study protocol and blind samples for determinations as well as testing materials necessary were shipped to each laboratory by AOAC Study Director in accordance with the guidelines of AOAC method evaluation.The collaborative laboratories tested the blind samples and sent back the analytical results to AOAC Study Director.The statistical results showed that two labs of them should be eliminated as they deviated from the protocol in some major operational procedures.For the remaining 14 labs：GC-MS/SIM（GC-MS/MS）：RSDr8% accounts for 100%,RSDR〈16% makes up 57.5%,RSDR〈25% accounts for 92.5%,HorRat values that are less than 1.0 account for 80.0%,HorRat values that are less than 2.0 account for 97.5%;LC-MS/MS：RSDr8% accounts for 65.0%,RSDr15% makes up 97.5%,RSDR16% accounts for 35.0%,RSDR25% makes up 95.0%,HorRat values that are less than 1.0 account for 92.5%,HorRat values that are less than 2.0 account for 97.5%.1 220 target pesticide calibration curves were established,1 132 with r^2 values satisfying the requirements of ≥0.995,making up 92.8%.Target ion abundance data were 3 600,3 443 is conforming to EU standard in abundance ratio,accounting for 95.6%.By these results,the method was proved to have good repeatability and reproducibility,and was suitable for the determination of multiple pesticide residues in tea.