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呋喃妥因肠溶片中有关物质检测及结构分析

ISSN号：0254-1793
期刊名称：《药物分析杂志》
时间：0
分类：R917[医药卫生—药物分析学;医药卫生—药学]
作者机构：[1]陕西省食品药品检验所,西安710061, [2]中国食品药品检定研究院,北京100050, [3]中国医学科学院药物研究所,北京100050
相关基金：国家卫生公益性行业科研专项基金（200902008）

关键词：呋喃妥因片, 有关物质, 水解产物杂质, 硝基糠醛二乙酯, 呋喃西林, 高效液相色谱法, 液质联用技术, nitrofurantion tablets , related substances , hydrolysate impurity , 5 - nitro furfural diacetate , nitrofura- zone , HPLC , LC - ESI - MS

中文摘要：

目的：分别建立呋喃妥因肠溶片中硝基糠醛二乙酯和呋喃西林、水解产物杂质A的HPLC测定方法，并采用液质联用技术对共性未知杂质进行结构分析。方法：PhenomenexC18色谱柱（250mm×4.6mm，5μm），测定硝基糠醛二乙酯的流动相为：磷酸盐缓冲液（取KH：PO4 6．8g，加水500mL，用磷酸调pH至4．5）-乙腈（50：50），检测波长306nm；测定呋喃西林、水解产物杂质A的流动相为：磷酸盐缓冲液（取KH2PO4 6．8g，加水500mL，用磷酸调pH至4．5）-乙腈（90：10），检测波长为365nm。结果：样品中各成分的分离度及检出灵敏度能满足有关物质限度的要求。硝基糠醛二乙酯的检出限为1．5ng，呋喃西林和杂质A的检出限分别为0．08ng、0．14ng。结论：建立的HPLC测定方法灵敏、准确、专属性强，适用于呋喃妥因片中有关物质的测定；采用液质联用技术初步推测出了未知杂质1的结构。

英文摘要：

Objective： To develop an HPLC method for the identification of 5 - nitro furfural diaeetate, nitrofurazone and substance A in nitrofurantion enteric - coated tablets, and to do structure analysis of common unknown sub- stances by LC -ESI -MS. Methods：A phenomenex C18 column for 5 -nitro furfural diacetate determination was a- dopted with a mobile phase consisting of phosphate buffer（ adjusted to pH 4.5 with 6. 8 g KH2PO4 added with 500 mL water） - acetonitrile （50： 50）,and the detection wavelength was 306 nm. The mobile phase of nitrofurazone and substance A consisted of phosphate buffer（ adjusted to pH 4. 5 with 6. 8 g KH2PO4added with 500 mL water） - acetonitrile （90： 10）, and the detection wavelength was 365 nm. Results： The resolution and sensitivity of related substances were acceptable. The detected limit of 5 - nitro furfural diaeetate was 1.5 ng, and the detected limits of nitrofurazone and substance A were 0. 08 ng and 0. 14 ng respectively. Conclusion：The method of HPLC is sensi- tive,accurate and specific to be used to determinate the related substances in nitrofurantion tablets;Initial structure of related substance 1 was inferred by LC -ESI- MS.

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