QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry

以QuEChERS作为样品前处理手段,建立测定水产品中扑草净残留的气相色谱-质谱法(GC-MS)。样品以乙腈-二氯甲烷(V∶V=8∶2)混合溶液提取,提取液经吸附剂中性氧化铝、N-丙基乙二胺(PSA)、纳米二氧化锆结合石墨化炭黑(GCB)净化后上机检测,内标法定量。结果显示,扑草净质量浓度介于5~200μg·L^(−1)线性关系良好,相关系数(R2)为0.9999。对草鱼(Ctenopharyngodon idellus)、鳜(Siniperca chuatsi)、中国对虾(Penaeus chinensis)、海参(Holothuria sp.)和文蛤(Meretrix meretrix)进行4个水平的加标回收实验(10、20、40和200μg·kg^(−1)),方法的加标回收率为85.8%~111.8%,相对标准偏差为1.2%~8.8%,满足GB/T 27404—2008《实验室质量控制规范食品理化检测》中实验室质量控制规范。扑草净的检出限(LOD,S/N≥3)和定量限(LOQ,S/N≥10)分别为5和10μg·kg^(−1)。该方法简单、快速、灵敏、净化效果好,能满足水产品中扑草净残留的检测需求。

A method was developed for the determination of prometryn in aquatic products by quick,easy,cheap,effective,rugged and safe(QuEChERS)extraction coupled with gas chromatography mass spectrometry.The samples were extracted by acetonitrile-dichloromethane mixture(V:V=8:2)and purified by neutral alumina,zirconium dioxide,PSA and GCB,quantified with internal standard.Good linearity was obtained in the range of 5.00−200μg·L^(−1)with the correlation coeficient of 0.9999.The average recoveries were 85.8%−111.8%in Ctenopharyngodon idellus,Siniperca chuatsi,Penaeus chinensis,Holothuria sp.and Meretrix meretrix at four spiked levels of 10,20,40 and 200μg·kg^(−1) with RSDS of 1.2%−8.8%,which meets the quality control specifications required in the national standard(GB/T 27404−2008 Criterion on Quality Control of Laboratories-Chemical Testing of Food).The limits of detection(S/N≥3)and quantification(S/N≥10)were 5.0 and 10.0μg·kg^(−1),respectively.The method is suitable for the rapid determination of the prometryn residues in aquatic products owing to its advantages of simplicity,sensitivity,accuracy and better purification.