液质联用法快速分析畜禽肉中的那西肽  

Rapid Analysis of Nosiheptide in Livestock and Poultry Meat by Liquid Mass Spectrometry

作　　者：贾江钢 范春蕾 张益 邹鲁 倪梅林 湛嘉 曹国洲 陈先锋 JIA Jiang-Gang;FAN Chun-Lei;ZHANG Yi;ZOU Lu;NI Mei-Lin;ZHAN Jia;CAO Guo-Zhou;CHEN Xian-Feng(Ningbo Zhongsheng Product Testing Co.,LTD.,Ningbo 315012;Ningbo Instituteof Inspectionand Quarantine Scienceand Technology,Ningbo 315012;Municipal Government of Meixian Town,Pingjiang County,Hunan Province,Yueyang 410412)

机构地区：[1]宁波中盛产品检测有限公司,宁波315012 [2]宁波检验检疫科学技术研究院,宁波315012 [3]湖南省平江县梅县镇政府,岳阳410412

出　　处：《中国口岸科学技术》2022年第11期67-71,共5页China Port Science and Technology

基　　金：宁波市创新团队重点专项(2015C110018);浙江省公益性基金(LGF21B050003)。

摘　　要：本文建立了畜禽肉中那西肽的简便快捷、可靠灵敏的检测方法。采用乙腈+二氯甲烷混合溶液匀浆提取,正己烷脱脂后,提取液氮吹至近干,用1 mol/L氢氧化钠在80℃下水解1 h后,正己烷再次脱脂,通过BEH C18色谱柱保留,获得良好的峰形,UPLC-MS/MS在电喷雾负离子模式下进行分析。优化后的前处理方法能充分去除复杂基质的干扰,特异性好,灵敏度高。定性检测限和定量检测限范围分别为2.5μg/kg和5μg/kg。基质添加曲线定量的线性良好,相关系数均不低于0.9950。对于鸡肉,3个添加水平的平均回收率分别为94.4%~108.6%,相应的变异系数分别为3.9%~8.3%,批间变异系数为4.5%,对于猪肉,3个添加水平的平均回收率分别为92.1%~111.1%,相应的变异系数分别为3.0%~5.5%,批间变异系数为3.4%。A rapid and simple analytical method able to identify nosiheptide in livestock and poultry meat was established.A mixture of acetonitrile and dichloromethane was used for homogenate extraction.After n-hexane degreasing,the extract was blown to near dry by nitrogen.After hydrolysis with 1 mol/L sodium hydroxide at 80℃for 1 h,n-hexane was degreased again,and retained by BEH C18column,a good peak shape was obtained.UPLC-MS/MS was analyzed in negative electrospray ionization mode.The results showed that the optimized pretreatment method could fully remove the interference of complex matrix with good specificity and sensitivity.The limit of quantitation(LOD)and the limit of quantification(LOQ)were 2.5μg/kg and 5μg/kg,respectively.The linearity of matrix-matched addition curves were no less than 0.9950.Average recoveries of the spiked chickens were in the range from 94.4%to 108.6%with associated RSD values from 3.9%to 8.3%.The inter-assay coefficient of variation was 4.5%.Average recoveries of the spiked pork were in the range from 92.1%to 111.1%with associated RSD values from 3.0%to 5.5%.The interassay coefficient of variation was 3.4%.

关 键 词：那西肽 前处理方法 液质联用 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]