硝酸甘油片有关物质方法的辅料扣除及质谱定性研究  

Identification and deduction ofexcipients in related substances of nitroglycerin tablets and qualitative spectrometry

作　　者：王琳[1] 余倩[1] 张喆[1] 郑洁[1] 古海锋[1] 车宝泉[1] 丛骆骆 

机构地区：[1]北京市药品检验所,北京100035 [2]北京市食品药品监督管理局,北京100053

出　　处：《药物分析杂志》2013年第11期1953-1957,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：北京市科技计划(Z111100074211021)

摘　　要：目的:建立液质联用法鉴别硝酸甘油片中的辅料,解决硝酸甘油片质量标准中有关物质辅料峰的判定和扣除问题。方法:采用Lichro CART C18色谱柱,流动相为乙腈-水(50∶50),大气压化学电离源,一级质谱全扫描,考察辅料峰的归属。通过重复性、稳定性和耐用性实验,以及水分的测定,考察辅料峰面积的稳定性。结果:样品色谱图中保留时间2.8min前的色谱峰为辅料峰,且该辅料峰在紫外检测和质谱检测中的响应值均主要源自聚维酮K 29/32。辅料峰的保留时间和峰面积均具有较好的重复性、稳定性和耐用性。扣除辅料峰后,3批硝酸甘油片样品的有关物质结果均符合规定。结论:本研究建立的液质联用法测定硝酸甘油片中的辅料,操作简单,结果准确,为相关辅料的研究提供了技术依据。根据辅料峰的归属和耐用性考察结果,为中国药典2010年版二部中硝酸甘油片质量标准修订提供了参考。To develop a new LC - MS method to determine the excipients in nitroglycerin tablets for the identification and deduction of exeipient peaks in related substances. Methods：The Lichro CART C18 column was used with acetonitrile -water as the mobile phase （50： 50）. A tandem mass spectrometer equipped with at- mospheric pressure chemical ionization source was used as the detector and was operated in full scan to quantify the excipients. An HPLC method and the water assay were used to investigate the stability of excipient area through repeatability, stability and ruggedness tests. Results：The peaks which were obtained before the retention time of 2. 8 min were judged as excipients in the ehromatograms of samples. The UV and MS response of the ex- cipient peak was mainly sourced from povidone K 29/32. The results of repeatability, stability and ruggedness tests were good in the retention time and peak area of samples. After deduction of the peaks of exeipients, the re- lated substance results of three batches of nitroglycerin tablets were all qualified in accordance with related re- quirements. Conclusion ： An accurate and feasible method based on LC - MS was developed to determine the ex- cipients in nitroglycerin tablets. According to the identification of exeipients and the results of ruggedness tests, the reference for revising the quality standards of nitroglycerin tablets in the 2010 edition of Chinese Pharmacopoeia was provided.

关 键 词：硝酸甘油片 高效液相色谱 质谱 有关物质 辅料 

分 类 号：R917[医药卫生—药物分析学]