水产品中磺胺类药物检测能力验证质量控制分析

Analysis on Quality Control of Proficiency Testing of Sulfonamides Determination in Aquatic Products

为保证实验室检验结果的准确性,参加了农业农村部组织的水产品中磺胺类药物检测能力验证活动,并对考核结果进行分析与经验探讨,以提高实验室检测能力。根据作业指导书要求,检测方法推荐使用《水产品中17种磺胺类及15种喹诺酮类药物残留量的测定液相色谱-串联质谱法》(农业部1077号公告-1-2008),对提取溶剂和净化方式进行优化,提取溶剂用乙腈代替标准中1%甲酸乙腈,磺胺类药物的响应得到明显提高,并用Oasis PRiME HLB固相萃取净化柱代替正己烷液液萃取除脂净化,将优化后建立的方法应用于本次水产品中磺胺类药物检测能力验证,取得了满意的实验结果。

In order to ensure the accuracy of laboratory test results,the proficiency testing activity of sulfonamides determination in aquatic products,organized by the Ministry of Agriculture and Rural Affairs,was participated in.Then the examination results to improve the laboratory detection ability were analyzed and discussed.According to the requirements of the operation instruction,“Simultaneous Determination of 17 Sulfonamides and 15 Quinolones Residues in Aquatic Products by LC-MS/MS Method”(Announcement No.1077-1-2008 of the Ministry of Agriculture)was recommended.The extraction solvent and purification method in this study were optimized as following,acetonitrile was used instead of 1%formic acid acetonitrile in the announcement,which improved significantly the response of sulfonamides,Oasis PRiME HLB solid phase extraction purification column was used to replace n-hexane liquid-liquid extraction for fat removal and purification.The optimized method was applied to the proficiency testing of sulfonamides determination in aquatic products,and the experimental results were satisfactory.