复方乙酰水杨酸片中有效成分的DOSY技术分析

doi:10.11938/cjmr20160306

波谱学杂志 ›› 2016, Vol. 33 ›› Issue (3): 415-421.doi: 10.11938/cjmr20160306

复方乙酰水杨酸片中有效成分的DOSY技术分析

王丽敏¹, 仇汝臣¹, 黄少华²

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

收稿日期:2015-10-08 修回日期:2016-07-10 出版日期:2016-09-05 发布日期:2016-09-05
通讯作者: 仇汝臣,电话:15314229751,E-mail:4969323@163.com;黄少华,电话:0532-80662660,E-mail:huangsh@qibebt.ac.cn. E-mail:4969323@163.com;huangsh@qibebt.ac.cn
作者简介: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.
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-min¹, QIU Ru-chen¹, HUANG Shao-hua²

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:2015-10-08 Revised:2016-07-10 Online:2016-09-05 Published:2016-09-05

摘要/Abstract

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.

关键词: 复方乙酰水杨酸片, 药物评价, 核磁共振(NMR), 二维扩散排序谱(DOSY), 二甲基硅油(PDMS)

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.

Key words: acetylsalicylic acid, pharmaceutical quality control, NMR, DOSY, polydimethylsiloxane (PDMS)

中图分类号:

O482.53

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.

WANG Li-min, QIU Ru-chen, HUANG Shao-hua. Quantitative Analysis of Active Ingredients in Compound Acetylsalicylic Acid Tablets by DOSY[J]. Chinese Journal of Magnetic Resonance, 2016, 33(3): 415-421.

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.

复方乙酰水杨酸片中有效成分的DOSY技术分析

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

PDF

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价

[1]	胡坤, 孙汉董, 普诺·白玛丹增. 量子化学计算核磁共振参数在天然产物结构鉴定中的应用[J]. 波谱学杂志, 2019, 36(3): 359-376.
[2]	尹田鹏, 王雅溶, 王敏, 石文智, 张正茜, 何莎莎. 三个C₁₉-二萜生物碱的NMR数据全归属[J]. 波谱学杂志, 2019, 36(3): 331-340.
[3]	杨云汉, 杜瑶, 应飞祥, 杨俊丽, 夏大真, 夏福婷, 杨丽娟. 柚皮素/β-环糊精超分子体系的包合行为[J]. 波谱学杂志, 2019, 36(3): 319-330.
[4]	王亚兰, 王晓静, 王志伟. 阿齐沙坦的波谱学数据及结构确证[J]. 波谱学杂志, 2019, 36(3): 350-358.
[5]	曹园, 吴永平, 陈东军. 卷柏属Selaginellin类化合物互变异构的波谱学研究[J]. 波谱学杂志, 2019, 36(2): 155-163.
[6]	寇新慧, 刘乙祥, 刘兴弘, 李从刚, 刘买利, 姜凌. 探测应答调控蛋白PhoB_N^F20D自由态中存在的Pre-Active构象[J]. 波谱学杂志, 2019, 36(2): 164-171.
[7]	陈晓瑛, 俞刚金, 毛诗珍, 刘买利, 杜有如. 利用¹H NMR探究混合离子型/非离子型表面活性剂临界胶束浓度降低的实质[J]. 波谱学杂志, 2019, 36(2): 219-224.
[8]	尹田鹏, 罗智慧, 蔡乐, 丁中涛. 天然C₁₉-二萜生物碱的研究进展及其核磁共振波谱特征[J]. 波谱学杂志, 2019, 36(1): 113-126.
[9]	冉梦琳, 覃凌云, 唐淳, 董旭. 磷酸化调控泛素单体与Rad23A/Ubiquilin-1中泛素结合域互作的检测[J]. 波谱学杂志, 2019, 36(1): 15-22.
[10]	魏会强, 于江, 毕常芬, 宁洪鑫, 李祎亮, 刘强. N-异丁酰基-3'-O-(1-氟-1,1,3,3-四异丙基-1,3-二硅氧烷-3-基)-2'-苄氧羰基鸟苷的NMR研究[J]. 波谱学杂志, 2019, 36(1): 93-102.
[11]	李英俊, 杨凯栋, 靳焜, 刘季红, 王思远, 张楠. 基于咔唑-靛红双-硫代碳酰腙衍生物的NMR研究[J]. 波谱学杂志, 2019, 36(1): 83-92.
[12]	迟秀娟, 乔晓亚, 刘颖, 刘惠丽, 陈雷, 王际辉, 艾选军. 拟南芥AtGrp7 RRM结构域的纯化及其结构与结合的初步分析(英文)[J]. 波谱学杂志, 2019, 36(1): 1-14.
[13]	尹田鹏, 汪泽, 陈阳, 邵娅婷, 邓亮, 黎唯. 10-吲哚细胞松弛素chaetoglobosin F的NMR解析[J]. 波谱学杂志, 2019, 36(1): 74-82.
[14]	王伟宇, 胡涵, 徐君, 邓风. Pd-Cu双金属催化剂上加氢反应的仲氢诱导超极化研究[J]. 波谱学杂志, 2018, 35(3): 269-279.
[15]	朱云峰, 何为, 何传红, 王怡, 齐天昊, 陈柏冰, 徐征. 基于数字调制技术的核磁共振射频脉冲发生器[J]. 波谱学杂志, 2018, 35(3): 318-327.