QuEChERS-超高效液相色谱-串联质谱法测定食品中7种糖皮质激素类兴奋剂药物残留  

Determination of Seven Glucocorticoid Residues of Stimulants in Food by QuEChERS Coupled with Ultra Performance Liquid Chromatography‐Tandem Mass Spectrometry

作　　者：姚晓庆 穆姝夷 李秀英 梁志森 YAO Xiaoqing;MU Shuyi;LI Xiuying;LIANG Zhisen(Guangzhou Inspection and Testing Certification Group Co.,Ltd.,Guangzhou 511447,Guangdong,China;National Quality Inspection and Testing Center for Processed Food(Guangdong),Guangzhou 511447,Guangdong,China)

机构地区：[1]广州检验检测认证集团有限公司,广东广州511447 [2]国家加工食品质量检验检测中心(广东),广东广州511447

出　　处：《食品研究与开发》2025年第8期211-217,共7页Food Research and Development

基　　金：中国认证认可协会科技计划项目(2022CCAAKY10)。

摘　　要：建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定食品中7种糖皮质激素类兴奋剂药物残留的分析方法。样品经乙腈涡旋提取,加入无水硫酸镁、氯化钠、柠檬酸钠和柠檬酸氢二钠盐析,提取液经N-丙基乙二胺(primary-secondary amine,PSA)吸附净化后,采用Accucore Biphenyl(100 mm×2.1 mm,2.6μm)色谱柱分离,以0.1%甲酸水-0.1%甲酸乙腈为流动相梯度洗脱,电喷雾离子源正离子(electron spray ionization+,ESI+)模式扫描,多反应监测模式(multiple responese monitoring,MRM)检测,外标法定量。7种糖皮质激素在0.1~100μg/L浓度范围内相关系数均大于0.999,线性关系良好,在低中高浓度水平的加标回收率为78.1%~118.5%,精密度为0.6%~14.7%。该方法适用于没有现行检测标准的7种糖皮质激素在食品中残留量的测定。This paper aimed to establish a method for determining seven glucocorticoid residues of stimulants in food by using QuEChERS coupled with ultra performance liquid chromatography⁃tandem mass spectrometry.The samples were extracted by acetonitrile vortex and salted out with anhydrous magnesium sulfate,sodium chloride,sodium citrate,and disodium hydrogen citrate.Then,the extraction solution was purified by primary⁃secondary amine(PSA).The samples were separated by Accucore Biphenyl(100 mm×2.1 mm,2.6μm)chro⁃matographic column,eluted with 0.1%formic acid⁃water solution and 0.1%formic acid⁃acetontrile solution as mobile phase,then scanned by electron spray ionization in positive mode,and detected by multiple response monitoring(MRM).The samples were quantified by an external standard method.The correlation coefficients of seven glucocorticoids were over 0.999 in the range of 0.1-100μg/L and had good linear relationships.The recoveries of seven glucocorticoids were 78.1%-118.5%at low,medium,and high concentrations,and the pre⁃cisions were 0.6%-14.7%.This method was suitable for the determination of seven glucocorticoid residues that were not clarified in existing standards in food.

关 键 词：QUECHERS 糖皮质激素 兴奋剂 超高效液相色谱-串联质谱法 兽药残留 

分 类 号：O657.7[理学—分析化学]