色谱2017，Vol.35Issue(6)：594-600,7.DOI:10.3724/SP.J.1123.2017.03007
超高效液相色谱-三重四极杆质谱法测定食品中34种非法添加减肥类化合物
Determination of 34 illegally adulterated weight loss compounds in foods by ultra high performance liquid chromatography-triple quadrupole mass spectrometry
摘要
Abstract
An analytical method was developed for the determination of 34 illegally adulterated weight loss compounds in foods and dietary supplements by ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS).A Waters CORTECS T3 column (100 mm×2.1 mm,2.7 μm) was used with 0.1% (v/v) formic acid aqueous solution-acetonitrile containing 0.1% (v/v) formic acid as mobile phases by gradient elution.The compounds were detected by electrospray ion source in positive or negative mode with multiple reaction monitoring (MRM) mode.The calibration curves showed good linearity in the range of 0.5-10 μg/L for 29 compounds such as sibutramine,and in the range of 2.5-50 μg/L for five compounds such as chlorothiazide.The correlation coefficients (r) of the standard calibration curves for the 34 analytes were all greater than 0.99.The recoveries of the 29 compounds at spiked levels of 5,10 and 20 μg/kg were in the range of 49.2%-136.2%,and the RSDs were 0.7%-15.0% (n=6).The recoveries of the five compounds at spiked levels of 25,50 and 100 μg/kg were in the range of 51.5%-130.9%,and the RSDs were 0.8%-14.0% (n=6).The limits of detection (LODs) and limits of quantification (LOQs) were 5 μg/kg and 10 μg/kg for the 29 compounds,25 μg/kg and 50 μg/kg for the five compounds,respectively.The method was successfully applied to the analysis of actual samples,and 12 compounds were checked out,which combated the illegal adulteration behavior effectively.关键词
超高效液相色谱-三重四极杆质谱/非法添加/减肥类化合物/食品Key words
ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS)/illegal adulteration/weight loss compounds/foods分类
化学化工引用本文复制引用
胡青,孙健,冯睿,张甦,于泓,张静娴,毛秀红,季申..超高效液相色谱-三重四极杆质谱法测定食品中34种非法添加减肥类化合物[J].色谱,2017,35(6):594-600,7.基金项目
上海市科委技术平台专项(14DZ2294000) （14DZ2294000）
2016年国家食品药品监督管理总局食品补充检验方法项目.Platform Project of Science and Technology Commission of Shanghai Municipality (No.14DZ2294000) （No.14DZ2294000）
2016 Food Detection Supplementary Method Development Project of the State Food and Drug Administration. （）
