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

发布时间：2018-02-28 23:27

本文关键词： 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　出处：《色谱》2017年06期 　论文类型：期刊论文

【摘要】：建立了超高效液相色谱-三重四极杆质谱测定食品(含保健食品)中34种减肥类非法添加化合物的方法。采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7μm),以0.1%(v/v)甲酸水溶液-含0.1%(v/v)甲酸的乙腈溶液为流动相,梯度洗脱,在电喷雾离子源、正离子或负离子模式下以多反应监测(MRM)方式检测。西布曲明等29种化合物在0.5~10μg/L范围内、氯噻嗪等5种化合物在2.5~50μg/L范围内均呈良好的线性关系,相关系数(r)均大于0.99;西布曲明等29种化合物在5、10和20μg/kg添加水平下的平均加标回收率为49.2%~136.2%,相对标准偏差(RSD)为0.7%~15.0%(n=6),氯噻嗪等5种化合物在25、50和100μg/kg添加水平下的平均加标回收率为51.5%~130.9%,RSD为0.8%~14.0%(n=6);西布曲明等29种化合物的检出限为5μg/kg,定量限为10μg/kg,氯噻嗪等5种化合物的检出限为25μg/kg,定量限为50μg/kg。本方法已应用于实际样品的测定,共检出了12种化合物,有效打击了非法添加行为。
[Abstract]:An ultra-high performance liquid chromatography-quadrupole mass spectrometry method for the determination of 34 kinds of weight-loss compounds in food (including health food) was established. The Waters CORTECS T3 column was used to determine the content of 0.1 渭 m 脳 2.1mm-1 渭 m of formic acid in aqueous solution of formic acid-containing 0.1% v / v) formic acid. Acetonitrile solution is a mobile phase. Gradient elution was performed in electrospray ion source, positive ion or negative ion mode, and MRM was used to detect 29 compounds such as sibutramine in the range of 0.5 ~ 10 渭 g / L and 5 compounds such as chlorothiazide in the range of 2.5 ~ 50 渭 g / L. The average recoveries of 29 compounds, such as sibutramine, etc., were 49.2% and 136.2 渭 g / kg, respectively, and the relative standard deviation (RSDs) were 0.710 and 100 渭 g / kg, respectively. The average recoveries of 29 compounds, such as sibutramine and chlorothiazide, were increased at 2550 and 100 渭 g / kg, respectively. The detection limits of sibutramine, sibutramine and chlorothiazide were 5 渭 g / kg, 10 渭 g / kg, 25 渭 g / kg and 50 渭 g / kg, respectively. A total of 12 compounds were detected, which effectively cracked down on the illegal addition behavior.
【作者单位】：上海市食品药品检验所;
【基金】：上海市科委技术平台专项(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~~
【分类号】：O657.63;TS207.3

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