摘要
建立了利用气相色谱-串联质谱检测平菇中666、五氯硝基苯等36种农药残留及其残余代谢物的检测方法。该方法克服了Qu ECh ERS方法对样品制备的破壁和即时冷冻要求,与固相萃取方法相比可节约溶剂,提高前处理效率。该方法采用乙腈提取平菇中的36种农药残留,以N-丙基乙二胺为主要材料对样品进行净化,用电喷雾电离,多反应模式检测,采用基质标准溶液外标法定量。研究表明:平菇中36种农药残留的含量重复性试验相对标准偏差2.47%~5.04%,定量限0.000 3~0.010 0 mg/kg,检出限0.000 09~0.004 00 mg/kg。36种农药及其残余代谢物在0.05~2.00 mg/L范围内线性关系良好,r值均> 0.990。按照不确定度评定方法,从标准溶液稀释、样品称量、样品最终定容体积和仪器测定重复性等方面对测量结果的测量不确定度进行评价,评价结果显示,测定结果不确定度主要来源于标准溶液。
An analytical method was developed for determination of 36 pesticide residues(666、quintozene and its residual metabolites)in oyster mushroom by gas chromatography-tandem mass spectrometry method.This method overcame demand for breaking and instant freezing by QuEChERS method,and more efficient and economical than solid phase extraction.The method were extracted with acetonitrile,further clean-up with N-Propylethylenediamine,determined in modes of electrospray ionization and multiple reaction monitoring,quantified by matrix standard solution external standard method.Results showed that relative standard deviations of 36 pesticide residues content was 2.47%~5.04%under this method for determination.The limits of quantification were 0.0003~0.0100 mg/kg,and limits of detection were 0.00009~0.00400 mg/kg.36 pesticides had a good linearity was obtained from range 0.05~2.00 mg/L and the r values were greater than 0.990.According to uncertainty evaluation method,items constituting measurement uncertainty involved standard dilution solution,weighing of sample,final volume of sample,and measurement repeatability of equipment were evaluated.Results showed that measurement uncertainty was mainly due to standard solution.
作者
王洁莲
张建新
王娜娜
WANG Jielian;ZHANG Jianxin;WANG Nana(Agricultural Products Quality Safety Monitoring Center of Shanxi Province,Taiyuan Shanxi 030025,China)
出处
《农业工程》
2021年第2期75-80,共6页
AGRICULTURAL ENGINEERING
关键词
平菇
农药残留
气相色谱-串联质谱法
不确定度
oyster mushroom
pesticide residues
gas chromatography-tandem mass spectrometry
uncertainty
