HPLC-MS/MS 检测中药制剂及保健食品中添加 6 种减肥药物的研究

曾祥林 ;何颂华 ;黄晓东 ;曾智

中国药学杂志 ›› 2009, Vol. 44 ›› Issue (17) : 1339-1342.

PDF(2444 KB)
PDF(2444 KB)
中国药学杂志 ›› 2009, Vol. 44 ›› Issue (17) : 1339-1342.
论文

HPLC-MS/MS 检测中药制剂及保健食品中添加 6 种减肥药物的研究

  • 曾祥林 1 ,何颂华 1 ,黄晓东 2 ,曾智 3
作者信息 +

Identification of Six Anti-obesity Chemical Drugs Added into Traditional Chinese Medicines and Health Foods by Liquid Chromatography-Ion Trap Mass Spectrometry Method

  • ZENG Xiang-lin 1 , HE Song-hua 1 , HUANG Xiao-dong 2 , ZENG Zhi 3
Author information +
文章历史 +

摘要

目的 建立专属、灵敏的 HPLC-MS/MS 方法甄别中药制剂及保健食品中可能添加的氯噻嗪、盐酸西布曲明、酚酞、吲哒帕胺、布美他尼、吉非罗齐等 6 种化学减肥药物。 方法 样品经甲醇提取, 采用液相色谱 - 离子阱质谱联用法测定。色谱条件: Inertsil ODS-3 色谱柱 (4.6 mm × 250 mm , 5 m m) ,梯度洗脱: 流动相 A 为 0.1% 醋酸溶液;流动相 B 为乙腈, 质谱条件:离子源 ESI , 选择正负离子全扫描、选择离子监测 (SIM) 、多反应监测 (MRM) 方式检测临床常用的 6 种化学减肥药物,研究了这 6 种药物的质谱裂 解规律。 通过比较样品峰与对照品峰的相对分子质量、二级质谱碎片信息和液相色谱保留时间,确定样品中是否违法添加了化学药物 。 结果 应用本法 检测了 12 批市售减肥类中药制剂及保健食品 , 其中 1 种减肥保健食品中检出西布曲明及酚酞, 1 种减肥保健食品中检出西布曲明,另外 2 种减肥保健食品检出酚酞 。 结论 该法 简便、快捷,灵敏度高、 专属性强,可作为 检测中药制剂及保健食品中非法掺入减肥类化学药的有效手段 。

Abstract

OBJECTIVE To develop a specific, sensitive and rapid HPLC-MS/MS method for the identification of 6 anti-obesity chemical drugs added illegally into Traditional Chinese Medicines and health foods. METHODS The liquid chromatography-ion trap mass spectrometry method with an electrospray ionization (ESI) source was used to separate and identify chlorthiazide, sibutramine, phenolphthalein, indapamide, bumetanide and gemfibrozi. The separation was performed on a Inertsil ODS-3 C18 column (4.6 mm×250 mm, 5 mm) with a gradient elution. The mobile phase was consisted of acetonitrile and 0.1% acetic acid at a flow rate of 0.7 mL·min-1. The mass spectrometer (Agilent 1100 series LC/MSD Trap SL) was operated in the positive ion or negative ion mode and in three scan modes including full scan MS, selected ion monitoring and full scan MS2. The obtained mass spectra were analyzed for their fragmentation passways. The obtained pseudomolecular ions, fragmentions and retention time were used to identify the six chemical drugs in traditional Chinese medicines and health foods. RESULTS It was found that sibutramine and phenolphthalein were illegally mixed into one health foods, sibutramine was illegally mixed into one health foods, phenolphthalein was illegally mixed in the other two health foods. CONCLUSION The method is specific and sensitive, can be used to identify traditional Chinese medicines and health foods, illegally adulterated by the anti-obesity drugs.

关键词

减肥药 / 氯噻嗪 / 西布曲明 / 酚酞 / 吲哒帕胺 / 布美他尼 / 吉非罗齐 / 高效液相色谱 - 质谱联用法

Key words

anti-obesity drugs / chlorthiazide / sibutramine / phenolphthalein / indapamide / bumetanide / gemfibrozi / HPLC-MS/MS

引用本文

导出引用
曾祥林 ;何颂华 ;黄晓东 ;曾智 . HPLC-MS/MS 检测中药制剂及保健食品中添加 6 种减肥药物的研究[J]. 中国药学杂志, 2009, 44(17): 1339-1342
ZENG Xing-lin;HE Song-hu;HUNG Xio-dong;ZENG Zhi . Identification of Six Anti-obesity Chemical Drugs Added into Traditional Chinese Medicines and Health Foods by Liquid Chromatography-Ion Trap Mass Spectrometry Method[J]. Chinese Pharmaceutical Journal, 2009, 44(17): 1339-1342

参考文献


[1] QIU Y H , WANG T J. Detection of phenolphthalein illegally mixed into slimming Chinese traditional medicines and health products by the liquid chromatography-quadrupole mass spectrometry method[J]. <>Chin J Pharm Anal ( 药物分析杂志 ) , 2006 , 26(11) : 1609-1611.
[2] GUO J F , CHEN X Y , ZHONG D F. Analysis of six anti-diabetics by liquid chromatography-mass spectrometry[J]. <>J Instrum Anal ( 分析测试学报 ) , 2000 , 19(6) : 5-8.
[3] WANG K , HU Q , CUI Y L. Detection of 28 chemical drugs added illegally into slimming traditional Chinese medicines and health food by liquid chromatography-ion trap mass spectrometry method[J]. <>Chin J Pharm Anal ( 药物分析杂志 ) , 2008 , 28(8) : 1268-1275.
[4] DAI J Y , LAI Z F. Determination of hydrochlorothiazide tablets by HPLC[J]. <>China Pharm ( 中国药师 ) , 2005 , 8(8) : 651-652.
[5] CAO W D , YU J W , GUAN L , <> et al . Determination of the content of sibutramine hydrochloride in Qumei Capsule by HPLC[J]. <>J China Pharm (中国药房), 2004 , 15(4) : 240-241.
[6] QIU Y H , LI M F , WANG T J. Determination of Chlorothiazide Tablet by HPLC[J]. <>China Pharm ( 中国药师 ) , 2005 , 8(11) : 966-967.
[7] ZHUANG L L , CHEN X D. Determination of content and content uniformity of Indapamide Tablet by HPLC[J]. <>J <>China Clin Med Res( 中华临床医学研究杂志 ) , 2006 , 12(2) : 162-163.
[8] RUAN B Q. Determination of Bumetanide Tablets by HPLC[J]. <>Strait Pharm J ( 海峡药学 ) , 2006 , 18(1) : 77-78.
[9] LI Y L , KAN X L , LI Q S. Determination of Gemfibrozil Capsule by HPLC[J]. <>J Shanxi Med Univ ( 山西医科大学学报 ) , 2001 , 32(4) : 316-317.
( 收稿日期 : 2009-03-10 )


PDF(2444 KB)

Accesses

Citation

Detail

段落导航
相关文章

/