QuEChERS/高效液相色谱-串联质谱法测定动物源性食品中14种蛋白同化激素残留  

Determination of 14 Anabolic Androgenic Steroids in Animal Derived Foods by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王敬 张海超 贾海涛 艾连峰 WANG Jing;ZHANG Haichao;JIA Haitao;AI Lianfeng(Technology Center of Shijiazhuang Customs,Shijiazhuang 050051,China)

机构地区：[1]石家庄海关技术中心,河北石家庄050051

出　　处：《食品工业科技》2022年第20期291-299,共9页Science and Technology of Food Industry

基　　金：河北省技术创新引导计划项目(21475501D);总署科技计划项目(2019HK112)。

摘　　要：建立了动物源性食品中群勃龙、勃地龙和诺龙等14种蛋白同化激素残留量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。试样加乙酸铵缓冲溶液,β-葡萄糖醛酸酶及芳香基硫酸酯酶酶解,酶解液经20 mL乙腈提取,取10 mL上清液经10 mL乙腈饱和正己烷除脂,以50 mg C_(18)、50 mg PSA和300 mg中性氧化铝吸附剂(含300 mg MgSO_(4))净化,使用C_(18)色谱柱分离,乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,正离子电喷雾多反应监测模式测定,基质匹配外标法定量。结果表明,目标化合物在0.1~10 ng/mL范围内线性相关系数均大于0.992,方法的检出限为0.3μg/kg,定量限为1.0μg/kg;采用1.0、2.0和10μg/kg添加水平的回收率范围为75.7%~104.1%,相对标准偏差(RSD)为3.60%~12.1%。方法简便快速,灵敏度高、重现性好,能够满足冬奥会食源性兴奋剂中常见蛋白同化激素残留量的快速检测需求。A method was developed for the determination of 14 anabolic androgenic steroids including trenbolone,boldenone and nandrolone in animal derived foods by liquid chromatography-tandem mass spectrometry.The samples were added to ammonium acetate buffer and enzymatic hydrolyzed byβ-glucuronidase and arysulfatase.The hydrolyzates were extracted with 20 mL acetonitrile,and then 10 mL supernatant was degreased by 10 mL acetonitrile saturated hexane,purified with 50 mg C_(18),50 mg PSA and 300 mg neutral alumina powder including 300 mg MgSO_(4).Then the analytes were separated by C_(18) column with gradient elution using 0.1% formic acid and acetonitrile as the mobile phase,detected in positive multiple reaction monitoring(MRM)and quantified with matrix-matched external standards.The linear regression correlation coefficients for the compounds were all higher than 0.992 in the range from 0.1 to 10 ng/mL.The limits of detection and the limits of quantification were 0.3 and 1.0μg/kg respectively.The recoveries at the addition levels of 1.0,2.0 and 10μg/kg were in the range of 75.7%~104.1%,with relative standard deviations(RSDs)of 3.60%~12.1%.This method had high effectivity,good reproducibility,simple operation and high efficiency,and could be used for the rapid determination needs of common anabolic androgenic steroids in foodborne stimulants in the Winter Olympic Games.

关 键 词：液相色谱-串联质谱 蛋白同化激素 QUECHERS 动物源性食品 

分 类 号：O657.7[理学—分析化学]