《分析方法目的的适宜性》在农药残留检测领域的应用  

Application of The fitness for purpose of analytical methods in the field of analyzing pesticide residues

作　　者：李丽[1] 周洪斌[2] 王现平 LI Li;ZHOU Hong-Bin;WANG Xian-Ping(Mechatronics Engineering Faculty of Zhenjiang Vocational Technical College,Jiangsu Union Technical Institute,Zhenjiang Branch,Zhenjiang 212000,China;Technology Center of Zhenjiang Entry-Exit Inspection and Quarantine Bureau,Zhenjiang 212008,China)

机构地区：[1]江苏联合职业技术学院镇江分院镇江高等职业技术学校机电工程系,镇江212000 [2]镇江出入境检验检疫局技术中心,镇江212008

出　　处：《食品安全质量检测学报》2019年第1期268-274,共7页Journal of Food Safety and Quality

基　　金：江苏省第十三批"六大人才高峰"高层次人才选拔培养资助计划项目(XCL-146)~~

摘　　要：目的以液相色谱-串接质谱联用仪(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测茶叶中丙草胺为例,按照欧盟《分析方法目的的适宜性》(以下称指南)进行方法确认。方法茶叶中的丙草胺用乙腈提取,经过石墨化炭黑和N-丙基乙二胺净化后,用液相色谱-串接质谱联用仪检测。结果目标化合物在0.039～0.625μg/L范围内线性关系良好,相关系数(r2)大于0.999。茶叶中丙草胺的定量限(LOQm)和检出限(LODm)分别为0.045、0.015μg/kg。不同加标浓度样品(LOQ、2LOQ、10LOQ)的平均回收率为90.0%～102.0%。重复性相对标准偏差为2.71%;中间精密度相对标准偏差为3.67%。结论本研究简化了样品前处理的方法,按照《指南》定义的9项要素对更改后的方法进行确认,并介绍了具体步骤。相关的检测结果均符合《指南》的要求,为单个实验室的方法确认和标准操作程序的编制提供参考。Objective Taking the analysis of pretilachlor in tea by use of liquid chromatography-tandem mass spectrometry(LC-MS/MS) as example,to carried out method validation in light of the Eurachem Guide-The fitness for purpose of analytical methods(referred as The Guide).Methods Pretilachlor in tea was extracted with acetonitrile.After purification with graphitized carbon black(GCB) and N-propylethylenediamine(PSA),pretilachlor in the extraction was determined by LC-MS/MS.Results The calibration curve showed a good linearity in the ranges of 0.039-0.625 μg/L with the correlation coefficient greater than 0.999(r2>0.999).The limit of quantification(LOQm) and limit of detection(LODm) were 0.045 and 0.015 μg/kg,respectively.The average recoveries varied from 90.0% to 102.0% at 3 spiked levels(LOQ,2 LOQ and 10 LOQ) with the relative standard deviations of 2.71%(repeatability) and of 3.67%(intermediate precision).Conclusion This study simplified the method of sample pretreatment,confirmed the modified method according to the 9 elements defined in The Guide,and introduced the specific steps.The relevant test results are in line with the requirements of The Guide,which can provide a reference for method validation in single lab and the draft of standard operating procedures in labs.

关 键 词：实验室方法确认指南 液相色谱-串接质谱仪 丙草胺 

分 类 号：O657.63[理学—分析化学] TQ450.263[理学—化学]