固相萃取-液相色谱串联质谱法测定奶及奶粉中12种同化激素药物残留量  

Determination of twelve anabolic steroids residues in milk and milk powders by SPE-LC-MS/MS

作　　者：赵善贞 杨惠琴 伊雄海 郭德华 盛永刚 封卓然 ZHAO Shanzhen;YANG Huiqin;YI Xionghai;GUO Dehua;SHENG Yonggang;FENG Zhuoran(Technic for Animal Plant and Food Inspection and Quarantine,Shanghai Customs,Shanghai 200135,China)

机构地区：[1]上海海关动植物与食品检验检疫技术中心,上海200135

出　　处：《分析试验室》2025年第1期55-60,共6页Chinese Journal of Analysis Laboratory

基　　金：“科技创新行动计划”技术标准项目(21DZ2208500);海关总署科研项目(2021HK192);上海市出入境食品和饲料检测专业技术服务平台项目(20DZ2291900)资助。

摘　　要：建立了奶及奶粉中12种同化激素多残留的固相萃取净化-液相色谱串联质谱(SPE-LC-MS/MS)检测方法。样品经乙腈提取、HLB固相萃取柱净化、氮气吹干后,残留物用乙腈:水(50:50,V/V)溶解定容,LCMS/MS多反应监测(MRM)模式测定,内标法定性定量分析。12种同化激素的检出限(LOD)均为0.5μg/kg,定量限(LOQ)均为1.0μg/kg。在1.0,2.0和10.0μg/kg添加水平下,12种同化激素在牛奶基质中的回收率在71.4%~109.0%之间;在羊奶基质中的回收率在72.9%~121.5%之间;在牛奶粉基质中的回收率在67.4%~113.0%之间,相对标准偏差(RSD)均<15%。该方法可应用于奶及奶粉中甲睾酮、表睾酮、诺龙、勃地龙、群勃龙、脱氢表雄酮、甲地孕酮、甲羟孕酮、醋酸甲地孕酮、醋酸甲羟孕酮、醋酸美仑孕酮、醋酸氯地孕酮等同化激素的定性定量分析。A rapid solid phase extraction-liquid chromatography tandem mass spectrometry(SPE-LC-MS/MS)method was established to determine the multiple residues of 12 anabolic steroids in milk and milk powders.The samples were extracted by acetonitrile,purified by an HLB solid phase extraction column,dried by nitrogen,and dissolved with acetonitrile:water(50∶50,V/V)for metered volume.LC-MS/MS was used in multiple reaction monitoring(MRM)mode for qualitative and quantitative analysis.The limit of detection(LOD)and limit of quantitation(LOQ)of the method were 0.5μg/kg and 1.0μg/kg,respectively.At the spiked levels of 1.0,2.0 and 10.0μg/kg,the recoveries were from 71.4%to 109.0%in cow milk,from 72.9%to 121.5%in goat milk,and from 67.4%to 113.0%in milk powder,with the relative standard deviations(RSDs)lower than 15%.This method can be applied to the qualitative and quantitative analysis of methyltestosterone,epitestosterone,nandrolone,boldenon,trenbolone,dehydroepiandrosterone,megestrol,medroxyprogesterone,megestrol acetate,medroxyprogesterone acetate,melengestrol acetate,and chlormadinone acetate in milk and milk power.

关 键 词：液相色谱串联质谱法(LC-MS/MS) 奶及奶制品 同化激素 

分 类 号：O657.63[理学—分析化学]