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山东大学学报(医学版) ›› 2009, Vol. 47 ›› Issue (12): 138-140.

• 论文 • 上一篇    

HPLC/MS/MS法测定抗风湿中药制剂中糖皮质激素类化学药

黄萍,凌霄   

  1. 山东省药品检验所, 济南 250101
  • 收稿日期:2009-09-10 出版日期:2009-12-16 发布日期:2009-12-16
  • 作者简介:黄萍(1962- ),女,副主任药师,研究方向为药物分析。

Detection of glucocorticosteroid in traditional Chinese preparation by the liquidchromatographymass spectrometry method

HUANG Ping, LING Xiao   

  1. Shandong Provincial Institute for Drug Control, Jinan 250101,China
  • Received:2009-09-10 Online:2009-12-16 Published:2009-12-16

摘要:

目的采用液相色谱-电喷雾离子阱质谱联用法(HPLC/MS/MS),以保留时间、结构和分子量信息为指标测定抗风湿、镇痛类中药制剂中可能添加的糖皮质激素类化学药醋酸泼尼松及泼尼松。方法建立HPLC/MS/MS 方法, 液相色谱: 色谱柱为Agilent C18柱,以0.01?mol/L甲酸铵溶液(甲酸调节pH值至4.0)-甲醇(30:70)为流动相, 流速0.4?mL/min,柱温30?℃, 检测波长270?nm;质谱: 电喷雾离子源正离子检测方式(ESI+),m/z范围50~1000,离子源喷射电压5?KV,雾化电压40?psi,干燥气温度350?℃,干燥气(N2)流速10?L/min,毛细管电压15?V。结果通过与对照品峰的保留时间及一级、二级质谱图谱比较,确定样品中是否添加了化学药。应用该法在供试品溶液中检出了醋酸泼尼松。结论该方法选择性强,可用于鉴别中药制剂中非法添加糖皮质激素类化学药醋酸泼尼松及泼尼松。

关键词: 中药制剂, 糖皮质激素, 液相色谱-质谱联用法

Abstract:

To identify prednisone acetate and prednisone of glucocorticoids chemical drugs added to traditional Chinese preparation of antirheumatic and analgesic by applying liquid chromatography coupled with electrospray ion trap mass spectrometry and taking retention time, chemical structure and molecular weight as indicators. MethodsThe detection was performed on a C18 column. The mobile phase consisted of 0.01?mol/L ammonium formate (adjusting pH to 4.0 with formic acid)methanol(30:70), flow rate was 0.4?mL/min, column temperature was 30?℃, and detection wavelength was 270?nm. The electrospray ionization source was applied and operated in positive ion mode(ESI+). The scanning rang was 501000?m/z, ionization voltage was 5 kV, nebulizer pressure was 40psi, drying gas temperature was 350?℃, flow rate was 10?L/min, and ion source sparging voltage  was 15?V. ResultsThe compounds illegally added into the traditional Chinese medicine were identified according to the spectrum, chromatogramphic behavior and mass spectral data by comparison with those of reference substances. ConclusionThe method is selective, sensitive and can be used to detect the illegally added components in traditional Chinese preparation and to control the preparation quality.

Key words: Traditional Chinese Preparation, Glucocorticosteroid, Liquid chromatographymass spectrometry

中图分类号: 

  • R917
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