液相色谱法同时测定复方制剂中川芎嗪和阿司匹林的含量

液相色谱法同时测定复方制剂中川芎嗪和阿司匹林的含量

王鹏, 齐美玲^*, 周莉, 方林

1.沈阳药科大学制药工程学院, 沈阳 110016;
2.北京理工大学理学院化学系, 北京 100081;
3.沈阳华泰药物研究所, 沈阳 110016

收稿日期:2003-11-04 修回日期:2004-02-10 出版日期:2004-03-15 发布日期:2004-03-15
通讯作者: 齐美玲*

Simultaneous Determination of Tetramethylpyrazine and Aspirin in a New Compound Formulation by Liquid Chromatography

WANG Peng, QI Mei-ling^*, ZHOU Li, FANG Lin

1. School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, S henyang 110016, China;
2. Department of Chemistry, School of Science, Beijing Institute of Technology, Beijing 100081, China;
3. Shenyang Pharmtech Institute of Pharmaceuticals, Shenyang 110016, China

Received:2003-11-04 Revised:2004-02-10 Online:2004-03-15 Published:2004-03-15
Contact: QI Mei-ling*

摘要/Abstract

摘要： 目的建立一种反相液相色谱法用于新复方制剂中川芎嗪和阿司匹林含量的同时测定. 方法采用Diamonsil C18色谱柱, 以甲醇-1.5%醋酸(35:65,V/V, pH = 3.1)为流动相, 流速为1.0 mL·min^-1. 结果色谱测定可在12 min内完成. 苯甲酸为内标. 在标示量80-120%的范围内, 川芎嗪和阿司匹林的回收率范围分别为99.6-100.3%和99.9-101.3%. 川芎嗪和阿司匹林的线性范围分别为25.0-300.0 μg·mL^-1 (r = 0.9999, n = 5)和12.5-150.9 μg·mL^-1 (r = 0.9997, n = 5). 结论本法可用于复方制剂中川芎嗪和阿司匹林含量的同时测定.

关键词: 液相色谱法, 川芎嗪, 阿司匹林, 含量测定

Abstract: Aim To establish a reversed-phase liquid chromatographic (LC) method for simultaneous determination of tetramethylpyrazine (TMP) and aspirin in a new compound formulation. Methods Chromatographic separation of the two drugs was achieved on a Diamonsil C18 column, using a binary mixture of methanol-1.5% acetic acid (35:65, V/V, pH = 3.1) as mobile phase at a flow rate of 1.0 mL·min^-1. Results Separation was completed in less than 12 min.Benzoic acid was used as the internal standard.Recoveries at levels corresponding to 80 % to 120 % of the label claim of the formulation ranged from 99.6 to 100.3 % for aspirin and from 99.9 to 101.3% for TMP.The linear range was 12.6-150.9 μg·mL^-1 (r = 0.9997, n = 5) for aspirin and 25.0-300.0 μg·mL^-1 (r = 0.9999, n = 5) for TMP. Conclusion The method developed can be used for the simultaneous determination of TMP and aspirin in pharmaceutical preparations.

Key words: liquid chromatography, liquid chromatography, tetramethylpyrazine, tetramethylpyrazine, asp irin, asp irin, assay, assay

中图分类号:

R917

R927.2

Supporting: ^*Corresponding author. Tel.: 010-68912667; fax: 010-68913293

王鹏, 齐美玲^*, 周莉, 方林. 液相色谱法同时测定复方制剂中川芎嗪和阿司匹林的含量[J]. .

WANG Peng, QI Mei-ling^*, ZHOU Li, FANG Lin . Simultaneous Determination of Tetramethylpyrazine and Aspirin in a New Compound Formulation by Liquid Chromatography[J]. .

参考文献

[1] Chen KJ. Certain progress in the treatment of coronary heart disease with traditional medicinal plants in China [J]. Am J Chin Med, 1981, 9 (2): 193-196.
[2] Guo SK, Chen KJ, Qian ZH, et al. Tetramethylpyrazine in the treatment of cardiovascular and cerebrovascular diseases [J]. Planta Med, 1983, 47 (2): 89.
[3] Sheu JR, Kan YC, Hung WC, et al. Mechanisms involved in the antiplatelet activity of tetramethylpyrazine in human platelets [J]. Thromb Res, 1997, 88 (3): 259-270.
[4] Li M, Handa S, Ikeda Y, et al. Specific inhibiting characteristics of tetramethylpyrazine, one of the active ingredients of the Chinese herbal medicine “Chuanxiong”, on platelet thrombus formation under high shear rates [J]. Thromb Res, 2001, 104(1): 15-28.
[5] Tendera M, Wojakowski W. Role of antiplatelet drugs in the prevention of cardiovascular events [J]. Thromb Res, 2003, 110 (5/6): 355-359.
[6] Pawar D, Shahani S, Maroli S. Aspirin-the novel antiplatelet drug [J]. Hong Kong Med J, 1998, 4 (4): 415-418.
[7] Lincoff AM. Anticoagulant and antiplatelet drugs [J]. Cathet Cardio Interv, 2001, 54 (5): 514-520.
[8] Schror K. Antiplatelet drugs. A comparative review [J]. Drugs, 1995, 50 (1): 7-28.
[9] Liang CC, Hong CY, Chen CF, et al. Measurement and pharmacokinetic study of tetramethylpyrazine in rat blood and its regional brain tissue by high-performance liquid chromatography [J]. J Chromatogr B, 1999, 724 (2): 303-309.
[10] Lu K, Li HX and DingMY. Analysis of tetramethylpyrazine in Ephedrae herba by gas chromatography-mass spectrometry and high-performance liquid chromatography [J]. J Chromatogr A, 2000, 878 (1): 147-152.
[11] Sawyer M, Kumar V. A rapid high-performance liquid chromatographic method for the simultaneous quantitation of aspirin, salicylic acid, and caffeine in effervescent tablets [J]. J Chromatogr Sci, 2003, 41 (8): 393-397.
[12] Gandhimathi M, Ravi TK, Abraham A, et al. Simultaneous determination of aspirin and isosorbide 5-mononitrate in formulation by reversed phase high pressure liquid chromatography [J]. J Pharm Biomed Anal, 2003, 32 (6): 1145-1148.
[13] Ruiz-Medina A, Fernández-de Córdova ML, Ortega-Barrales P, et al. Flow-through UV spectrophotometric sensor for determination of acetylsalicylic acid in pharmaceutical preparations [J]. Int J Pharm, 2001, 216 (1/2): 95-104.
[14] Altun ML, Ceyhan T, Kartal M, et al. LC method for the analysis of acetylsalicylic acid, caffeine and codeine phosphate in pharmaceutical preparations [J]. J Pharm Biomed Anal, 2001, 25 (1): 93-101.
[15] Wang C, Vickers JT, Mann CK. Direct assay and shelf-life monitoring of aspirin tablets using Raman spectroscopy [J]. J Pharm Biomed Anal, 1997, 16 (1): 87-94.
[16] Kees F, Jehnich D, Grobecker H. Simultaneous determination of acetylsalicylic acid and salicylic acid in human plasma by high-performance liquid chromatography [J]. J Chromatogr B, 1996, 677 (1): 172-177.