SinChERS净化-气相色谱-质谱法快速测定畜肉中吲哚乙酸  

Rapid Determination of Indoleacetic Acid in Meat by Single-Step,Cheap,Effective,Rugged,and Safe(SinChERS)Purification Coupled with Gas Chromatography-Mass Spectrometry

作　　者：李霞 高喜凤 崔玉花 申中兰 陈倩倩 李芳芳 李海霞 徐大玮 李新玲 刘艳明 LI Xia;GAO Xifeng;CUI Yuhua;SHEN Zhonglan;CHEN Qianqian;LI Fangfang;LI Haixia;XU Dawei;LI Xinling;LIU Yanming(Industrial Technology Foundation Public Service Platform,Key Laboratory of Supervising Technology for Meat and Meat Products,State Administration for Market Regulation,Shandong Institute for Food and Drug Control,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院,国家市场监督管理总局重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,山东济南250101

出　　处：《肉类研究》2025年第4期11-16,共6页Meat Research

基　　金：国家市场监督管理总局科技计划项目(2022MK072)。

摘　　要：基于SinChERS净化-快速衍生化结合气相色谱-质谱法建立畜肉中吲哚乙酸的检测方法。样品加水后用甲酸调节pH值为3,采用乙腈提取,SinChERS净化柱净化,氮气吹干后加入浓硫酸、甲醇衍生化1 min,气相色谱-质谱法测定,基质外标法定量。结果表明,在0.01~5.0μg/mL范围内,吲哚乙酸质量浓度与其响应值线性关系良好,相关系数大于0.999。方法检出限为0.003 mg/kg,定量限为0.01 mg/kg。猪肉、牛肉、羊肉3种样品基质在0.01、0.05、0.10 mg/kg吲哚乙酸加标量下,平均加标回收率为92.1%~102.1%,相对标准偏差为2.6%~5.7%。该方法前处理时间短、灵敏度高、可用于畜肉中吲哚乙酸的快速测定。A method for the determination of indoleacetic acid in meat was established using a single-step,cheap,effective,rugged,and safe(SinChERS)purification and rapid derivatization followed by gas chromatography-mass spectrometry(GC-MS).After adding water and adjusting pH to 3 by formic acid,the samples were extracted with acetonitrile,purified on a SinChERS column,and blown to dryness under nitrogen.The residue was derivatized with concentrated sulfuric acid and methanol for 1 min prior to GC-MS analysis.Quantitative was performed using the matrix external standard method.The results showed that the linear relationship of indoleacetic acid concentration and its response value was good in the range of 0.01–5.0μg/mL,with a correlation coefficient(r2)greater than 0.999.The limit of detection was 0.003 mg/kg and the limit of quantification was 0.01 mg/kg.The average recoveries of pork,beef,and mutton samples spiked at 0.01,0.05,and 0.10 mg/kg were 92.1%to 102.1%,with relative standard deviations(n=6)of 2.6%to 5.7%.The method is characterized by high sensitivity and short pretreatment time,and can be used for the determination of indoleacetic acid in meat.

关 键 词：畜肉 吲哚乙酸 SinChERS 浓硫酸-甲醇 气相色谱-质谱法 

分 类 号：O657.63[理学—分析化学]