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减肥产品中非法添加西布曲明类似物的ESI-MS/MS检测与确证
引用本文:梁祈,黄文静,胡碧波,冯锐.减肥产品中非法添加西布曲明类似物的ESI-MS/MS检测与确证[J].分析测试学报,2013,32(5):609-613.
作者姓名:梁祈  黄文静  胡碧波  冯锐
作者单位:1. 广东省药品检验所,广东广州,510180
2. 广州中医药大学中药资源科学与工程研究中心,广东广州,510006
基金项目:广东省食品药品监督管理局资助项目(ZA20081207)
摘    要:通过分析西布曲明和减肥类健康产品中未知化合物质谱图的质谱信息,由高分辨串联质谱获得裂解碎片离子的精密质量数,质谱软件给出碎片的可能组成,推测了西布曲明和未知化合物的质谱裂解途径,进而推测出该化合物的结构。并通过合成该结构的化合物,采用液相色谱-串联质谱法对样品作确证检验,证实样品中添加了新的西布曲明类似物。该实验提供了一种可用于检测和确证健康产品中非法添加合成药物未知类似物的方法。

关 键 词:减肥产品  非法添加  西布曲明类似物  ESI-MS/MS检测和确证

ESI-MS/MS Detection and Verification of Sibutramine Analogues Adulterated in Slimming Products
LIANG Qi , HUANG Wen-jing , HU Bi-bo , FENG Rui.ESI-MS/MS Detection and Verification of Sibutramine Analogues Adulterated in Slimming Products[J].Journal of Instrumental Analysis,2013,32(5):609-613.
Authors:LIANG Qi  HUANG Wen-jing  HU Bi-bo  FENG Rui
Institution:1.Guangdong Provincial Institute for Food and Drug Control,Guangzhou 510180,China;2.Research Center of Chinese Herbal Resource Science and Engineering,Guangzhou University of Chinese Medicine,Guangzhou 510006,China)
Abstract:By analysis of mass spectra of sibutramine and an unknown compound in a health supplement for anti-obesity,this paper proposed the mass fragmentation pathways of sibutramine and the unknown compound,and deduced the structure of the unknown compound by piecing together fragments of the compound detected on a high-resolution mass spectrometry.The compound of the structure was synthesized and its structure was elucidated by analysis of elements,infrared spectrometry,mass spectrometry and nuclear magnetic resonance.With the synthesized compound as the reference substance,a verification examination of the sample was performed by HPLC-MS/MS.The results indicated that a new sibutramine analogue was adulterated in the sample.The study provided an effective strategy in detection and verification on analogues of synthesized drugs adulterated in health supplements.
Keywords:healthy products  illegal adulteration  sibutramine analogues  ESI-MS/MS detection and verification
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