摘要
建立通过式固相萃取-超高效液相色谱-串联质谱法测定食品中的曲美他嗪、氯米芬和美度铵残留量的方法。样品采用5%甲酸-乙腈提取,固相萃取小柱净化,经Amide色谱柱(3.0 mm×100 mm,1.7μm)分离后,在多反应监测模式下测定,内标法定量。氯米芬和曲美他嗪在1.0~40.0 ng/mL质量浓度范围内线性关系良好;美度铵在5.0~200.0ng/mL质量浓度范围内线性关系良好。测定结果相对标准偏差为0.3%~6.1%(n=6),平均加标回收率为81.3%~100.7%,该方法能有效降低基质干扰、简便快速、实用性强,普遍适用于食品中的氯米芬、曲美他嗪和美度铵的测定,可为体育赛事的食品保障工作提供有效的技术支撑。
In this study,we established a method for the determination of three metabolic regulators including clomiphene,trimetazidine and meldonium in foods by pass-through solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS).The samples were extracted with 5%formic acid in acetonitrile,and the extract was purified on a pass-through solid phase extraction column and chromatographically separated on an Amide column(3.0 mm×100 mm,1.7μm).The separated analytes were detected in the multiple reaction monitoring(MRM)mode,and quantitated by an internal standard method.Good linearity was observed for clomiphene and trimetazidine within the concentration range of 1.0-40.0 ng/mL,and 5.0-200.0 ng/mL for meldonium.The average recoveries for spiked samples ranged from 81.3%to 100.7%,and the relative standard deviations(RSD)were between 0.3%and 6.1%(n=6).The developed method was simple,rapid and practical with low matrix interferences,and was generally suitable for the determination of clomiphene,trimetazidine and meldonium in foods,which could provide effective technical support for the assurance of food safety for sports events.
作者
宋娟
李君
张阳阳
姚蕾珺
肖全伟
李绍波
戴琴
SONG Juan;LI Jun;ZHANG Yangyang;YAO Leijun;XIAO Quanwei;LI Shaobo;DAI Qin(Chengdu Institute of Food Inspection,Chengdu 611130,China;Key Laboratory of Chemical Metrology and Applications on Nutrition and Health for State Market Regulation,Beijing 100029,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2024年第8期257-264,共8页
Food Science
基金
“十四五”国家重点研发计划重点专项(2022YFF0710405)
国家市场监督管理总局项目(2021YJ009)
四川省科技计划项目(2022YFS0511)。
关键词
氯米芬
曲美他嗪
美度铵
超高效液相色谱-串联质谱法
固相萃取
clomiphene
trimetazidine
meldonium
ultra-high performance liquid chromatography-tandem mass spectrometry
solid phase extraction
