超高效液相色谱-串联质谱法检测畜肉及内脏中苯甲酸和马尿酸残留  

Determination of Benzoic Acid and Hippuric Acid Residues in Meat and Offal by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王娟强 刘梦瑶 张明悦 赵文涛[1] 李莹莹[1] 郭文萍[1] WANG Juanqiang;LIU Mengyao;ZHANG Mingyue;ZHAO Wentao;LI Yingying;GUO Wenping(China Meat Research Center,Beijing Key Laboratory of Meat Processing Technology,Beijing 100068,China)

机构地区：[1]中国肉类食品综合研究中心,肉类加工技术北京市重点实验室,北京100068

出　　处：《食品科学》2022年第14期311-318,共8页Food Science

基　　金：“十三五”国家重点研发计划重点专项(2017YFC1601706)。

摘　　要：建立超高效液相色谱-串联质谱技术对畜肉及内脏中苯甲酸和马尿酸进行检测。通过加标回收优化提取溶剂和净化方式,最终选择纯甲醇提取,经PRiME HLB固相萃取小柱净化,采用多反应监测模式检测,外标法定量。结果表明:苯甲酸在20~1000 ng/mL、马尿酸在4~200 ng/mL质量浓度范围内线性关系良好,线性相关系数均大于0.99,检出限分别为12.5μg/kg和2.5μg/kg,定量限分别为50μg/kg和10μg/kg;在3个添加水平的回收率在70.5%~99.7%之间,精密度相对标准偏差在0.3%~7.1%之间(n=6);方法具有良好的重复性和日内、日间稳定性,相对标准偏差不大于7.2%。该方法前处理简单、准确灵敏、回收率好,可为畜肉及内脏中苯甲酸和马尿酸残留量的监管提供技术支持。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of benzoic acid and hippuric acid in meat and offal.Through spiked recovery tests,methanol was selected as the extraction solvent.The extract was purified on a PRiME HLB solid phase extraction(SPE)column,detected in the multi-reaction monitoring(MRM)mode,and quantified by an external standard method.The results showed that good linearity was observed for benzoic acid and hippuric acid within the concentration range of 20-1000 and 4-200 ng/mL with correlation coefficients of greater than 0.99,and the detection limits 12.5 and 2.5μg/kg,respectively.The limits of quantification for benzoic acid and hippuric acid were 50 and 10μg/kg,respectively;the recoveries at three spiked concentration levels were between 70.5%and 99.7%,and the relative standard deviations(RSDs)of precision were 0.3%-7.1%(n=6).The proposed method had good repeatability and intra-and inter-day stability,with RSDs equal to or less than 7.2%.Therefore,this method is simple,accurate and sensitive,and has a good recovery rate.It can provide technical support for the supervision of benzoic acid and hippuric acid residues in meat and offal.

关 键 词：超高效液相色谱-串联质谱法 畜肉及内脏 苯甲酸 马尿酸 

分 类 号：TS201.6[轻工技术与工程—食品科学]