研究论文

复方乙酰水杨酸片中有效成分的DOSY技术分析

  • 王丽敏 ,
  • 仇汝臣 ,
  • 黄少华
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  • 1. 青岛科技大学 化工学院, 山东 青岛 266042;
    2. 中国科学院 青岛生物能源与过程研究所, 山东省合成生物学省级重点实验室, 山东 青岛 266101
王丽敏(1989-),女,山东聊城人,硕士研究生,主要从事化学分析及石油加工工作.

收稿日期: 2015-10-08

  修回日期: 2016-07-10

  网络出版日期: 2016-09-05

基金资助

国家自然科学基金资助项目(21105108).

Quantitative Analysis of Active Ingredients in Compound Acetylsalicylic Acid Tablets by DOSY

  • WANG Li-min ,
  • QIU Ru-chen ,
  • HUANG Shao-hua
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  • 1. School of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;
    2. Shandong Provincial Key Laboratory of Synthetic Biology, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266101, China

Received date: 2015-10-08

  Revised date: 2016-07-10

  Online published: 2016-09-05

摘要

复方乙酰水杨酸片是临床常用的解热镇痛消炎药物,目前其有效成分的分析方法存在操作繁琐而分析速度慢等不足. 该文利用二甲基硅油(PDMS)辅助的扩散排序(DOSY)技术以及扩散排序-同核相关(DOSY-COSY)联用技术,成功地对复方乙酰水杨酸片中三种有效成分的分子结构进行了快速定性分析,并且利用核磁共振氢谱(1H NMR)技术进行了相对定量分析. 该方法具有方便、快捷等特点,可作为借鉴和参考用于药物的质量评价.

本文引用格式

王丽敏 , 仇汝臣 , 黄少华 . 复方乙酰水杨酸片中有效成分的DOSY技术分析[J]. 波谱学杂志, 2016 , 33(3) : 415 -421 . DOI: 10.11938/cjmr20160306

Abstract

Compound acetylsalicylic acid tablet is a clinical drug having antipyretic, analgesic and anti-inflammatory effects. The present methods to analyze the active ingredients in this drug have many disadvantages. In this study, we used polydimethylsiloxane (PDMS)-assisted diffusion ordered NMR spectroscopy (DOSY), DOSY-correlated spectroscopy (COSY), and relative quantitative 1H NMR techniques to analyze the three main active ingredients in this drug. The content ratios among the 3 components could be obtained. It is argued that PDMS-assisted DOSY provides a convenient and efficient method for pharmaceutical quality control of compound acetylsalicylic acid tablets.

参考文献

[1] Shen Rong-bin(沈蓉滨). Pharmacology(药物学)[M]. Beijing(北京): Science Press(科学出版社), 2008: 117-121.

[2] China Pharmacopoeia Committee(国家药典委员会). Pharmacopoeia of the people's republic(中华人民共和国药典)[M]. Beijing(北京): Chemical Industry Press(化学工业出版社), 1997: 386.

[3] Wang Teng(王腾), Wang Xiao-min(王晓敏), Zhang Ya-yun(张亚运), et al. Simultaneous determination of three components in compound aspirin tablets by HPLC(高效液相色谱法同时测定复方乙酰水杨酸片中各有效成分的含量)[J]. Journal of Beijing Institute of Petro-chemical Technology(北京石油化工学院学报), 2012, 20(1): 41-44.

[4] Zhao Huai-qing(赵怀清), Wang Xue-ya(王学娅), Yang Li(杨丽), et al. Simultaneous determination of the contents of the three components in the APC by micellar thin layer chromatography(胶束薄层色谱法同时测定APC片中3组分含量)[J]. Journal of Shenyang Pharmaceutical University(沈阳药科大学学报), 2001, 18(5): 338-340.

[5] Sun Zeng-xian(孙增先), Zhang Qian-feng(张骞峰), Zhou Jin-yu(周金玉). Determination of three components in compound acetylsalicylic acid tablet by dual-wavelength ratio spectrometry(双波长比值光谱法测定复方乙酰水杨酸片中三组分含量)[J]. Spectros Spect Anal(光谱学与光谱分析), 2004, 24(7): 883-886.

[6] Zhou Qiu-ju(周秋菊), Xiang Jun-feng(向俊峰), Tang Ya-lin(唐亚林). Applications of nuclear magnetic resonance spectroscopy in drug discovery(核磁共振波谱在药物发现中的应用)[J]. Chinese J Magn Reson(波谱学杂志), 2010, 27(1): 68-79.

[7] Balayssac S, Trefi S, Gilard V, et al. 2D and 3D DOSY 1H NMR, a useful tool for analysis of complex mixtures: application to herbal drugs or dietary supplements for erectile dysfunction[J]. Pharm Biomed Anal, 2009, 50(4): 602-612.

[8] Trefi S, Routaboul C, Hamieh S. Analysis of illegally manufactured formulations of tadalafil (Cialis) by 1H NMR, 2D DOSY 1H NMR and Raman spectroscopy[J]. Pharm Biomed Anal, 2008, 47(1): 103-113.

[9] Li Shuang(李爽), Feng Xiu-yan(冯秀燕). A mini review on NMR approaches for coal analysis (NMR方法在煤炭分析中的应用进展)[J]. Chinese J Magn Reson(波谱学杂志), 2013, 30(1): 148-155.

[10] Johnson C S. Diffusion ordered nuclear magnetic resonance spectroscopy: Principles and applications progress in nuclear magnetic resonance[J]. Prog Nucl Magn Reson Spectrosc, 1999, 34(3, 4): 203-256.

[11] Cohen Y, Avram L, Frish L. Diffusion NMR spectroscopy in supramolecular and combinatorial chemistry: an old parameter—new insights[J]. Angew Chem Int Edit, 2005, 44(4): 520-554.

[12] Ito F, Hirabayashi S. Infrared spectra of the CF3I dimer: a concurrent application of matrix-isolation spectroscopy and cavity ring-down spectroscopy[J]. J Chem Phys, 2006, 124(23): 234509.

[13] Tormena C F, Evans R, Haiber S, et al. Matrix-assisted diffusion-ordered spectroscopy: mixture resolution by NMR using SDS micelles[J]. Magn Reson Chem, 2010, 48(7): 550-553.

[14] Tormena C F, Evans R, Haiber S, et al. Matrix-assisted diffusion-ordered spectroscopy: application of surfactant solutions to the resolution of isomer spectra[J]. Magn Reson Chem, 2012, 50(6): 458-465.

[15] Evans R, Haiber S, Nilsson M, et al. Isomer resolution by micelle-assisted diffusion-ordered spectroscopy[J]. Anal Chem, 2009, 81(11): 4 548-4 550.

[16] Chaudhari S R, Suryaprakash N. Diffusion ordered spectroscopy for resolution of double bonded cis, trans-isomers[J]. J Mol Struct, 2012, 1 017(23): 106-108.

[17] Wu Rui(吴瑞), Bai Zheng-wu(柏正武), Yang Ying(杨盈), et al. Study of the separation performance of PDMS matrixed chromatographic NMR technique(基于PDMS的NMR中色谱技术的分离性能研究)[J]. Chinese J Magn Reson(波谱学杂志), 2015, 27(1): 68-79.

[18] Huang S H, Gao J, Wu R, et al. Polydimethylsiloxane: a general matrix for high-performance chromatographic NMR spectroscopy[J]. Angew Chem Int Edit, 2014, 53(43): 11 592-11 595.

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