UPLC-MS/MS快速检测蛋及再制蛋中13种磺胺及甲氧苄啶  

Simultaneous determination of 13 sulfonamide and trimethoprim residues in eggs and reformed eggs by UPLC-MS/MS

作　　者：黄丽娟 李道霞 邵曼 李澍才 杜钢 余晓琴 HUANG Lijuan;LI Daoxia;SHAO Man;LI Shucai;DU Gang;YU Xiaoqin(Sichuan Institute of Food Inspection,Chengdu 610097;Key Laboratory of Baijiu SupervisionTechnology for State Market Regulation,Chengdu 610097)

机构地区：[1]四川省食品检验研究院,成都610097 [2]国家市场监管重点实验室(白酒监管技术),成都610097

出　　处：《中国食品添加剂》2024年第2期211-219,共9页China Food Additives

基　　金：国家重点研发计划项目(2017YFC1601300)。

摘　　要：建立UPLC-MS/MS法快速检测鲜蛋及再制蛋中13种磺胺类药物和甲氧苄啶残留的方法。样品经乙腈提取后,无水硫酸钠净化,氮气吹干复溶,正己烷除脂后得供试品。13种磺胺类药物和甲氧苄啶在0.5~50 ng/mL范围内相关系数r均高于0.9960,线性关系良好。方法检出限为0.2μg/kg,在添加水平2、5、10μg/kg时,回收率在76.6%~112.7%之间,相对标准偏差(n=6)均在7%以内。使用该方法检测100批鲜蛋和25批再制蛋,其中7批鲜蛋检出磺胺间甲氧嘧啶、甲氧苄啶、磺胺甲唑、磺胺喹啉,2批再制蛋检出磺胺间甲氧嘧啶和甲氧苄啶,含量范围为2.0~688.8μg/kg。该方法简便快速、准确可靠、灵敏度高、抗干扰力强,适用于鲜蛋和再制蛋中磺胺类药物和甲氧苄啶的快速检测。To establish a method for simultaneous determination of thirteen kinds of sulfonamide and trimethoprim residues in eggs and reformed egg products by ultrahigh-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),samples were extracted with acetonitrile,purified by anhydrous sodium sulfate,collected and dried with nitrogen,and redissolved and degreased.The results showed that the 13 compounds showed good linearity in the concentration range of 0.5~50 ng/mL,with correlation coefficients(r)greater than 0.996.The limits of detection were 0.2μg/kg,the recoveries were in the range of 76.6%~112.7%,with the relative standard deviations(n=6)less than 7%.This method was used to analyze 100 batches of eggs and 25 batches of reformed egg products.Sulfamonomethoxine,trimethoprim,sulfamethoxazole,and sulfaquinoxaline were detected in 7 batches of eggs,and trimethoprim and sulfamonomethoxine were detected in 2 batches of reformed egg products.The contents ranged from 2.0 to 688.8μg/kg.The developed method was simple,fast,sensitive,accurate,and strong in anti�interference,it is suitable for fast detection of sulfonamide and trimethoprim in eggs and reformed egg products.

关 键 词：超高效液相色谱-串联质谱 磺胺类化合物 甲氧苄啶 再制蛋 

分 类 号：TS207.3[轻工技术与工程—食品科学]