色谱 ›› 2014, Vol. 32 ›› Issue (1): 13-20.DOI: 10.3724/SP.J.1123.2013.08035

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱联用法同时检测降糖类和减肥类保健品中20种非法添加的化学降糖药物

朱峰, 阮丽萍, 马永建, 吉文亮, 刘华良   

  1. 江苏省疾病预防控制中心, 江苏 南京 210009
  • 收稿日期:2013-08-21 修回日期:2013-09-23 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 刘华良
  • 基金资助:

    江苏科技厅科技支撑计划项目(BE2010745);江苏省“十二五”科教兴卫工程项目(ZX201109).

Simultaneous determination of 20 illegally added anti-diabetic chemical components in hypoglycemic and weight-reducing health foods by ultra-high performance liquid chromatography-tandem mass spectrometry

ZHU Feng, RUAN Liping, MA Yongjian, JI Wenliang, LIU Hualiang   

  1. Jiangsu Provincial Center for Disease Prevention and Control, Nanjing 210009, China
  • Received:2013-08-21 Revised:2013-09-23 Online:2014-01-08 Published:2013-12-26

摘要:

建立了一种利用超高效液相色谱-质谱联用同时快速筛查、检测降糖类和减肥类保健品中20种非法添加化学成分的方法。试样用甲醇提取后,经Poroshell 120 EC-C18柱(100 mm×2.1 mm,2.7 μm)分离,以5 mmol/L乙酸铵和乙腈为流动相梯度洗脱,采用电喷雾离子源正、负离子模式切换、多反应监测模式检测。20种非法添加化合物的峰面积与质量浓度均呈良好的线性关系,相关系数均大于0.99,回收率均在75.9%~114.0%范围内,相对标准偏差均不高于11.3%,检出限均在0.3~1.5 μg/L范围内。该方法快速、简便、灵敏、重现性好,为打击降糖类和减肥类保健品中非法添加化学降糖药提供了有力的依据。

关键词: 保健品, 超高效液相色谱-质谱, 非法添加物, 化学降糖药物

Abstract:

A rapid method for the simultaneous screening and detection of 20 illegally added anti-diabetic chemical components in hypoglycemic and weight-reducing health foods was developed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After extracted by methanol, the sample was separated on a Poroshell 120 EC C18 column (100 mm×2.1 mm, 2.7 μm) with the gradient elution of 5 mmol/L ammonium acetate and acetonitrile as mobile phases. The electrospray ionization (ESI) source in positive or negative ion mode was used for multiple reaction monitoring (MRM) mode. The 20 illegally added chemical components showed good linear relationships with the correlation coefficients more than 0.99. The recoveries were in the range of 75.9%-114.0%, and the relative standard deviations (RSDs) were all not more than 11.3%. The limits of detection (LODs) were all in the range of 0.3-1.5 μg/L. This method is rapid, simple, sensitive, accurate and of good specificity for cracking down illegally added anti-diabetic chemical components.

Key words: anti-diabetic chemical drugs, health foods, illegal additives, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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