HPLC法测定富马酸二甲酯有关物质Determination of related substances of dimethyl fumarate by HPLC
于小涵,周现滢,安珍珍,于治国
YU Xiao-han,ZHOU Xian-ying,AN Zhen-zhen,YU Zhi-guo
摘要(Abstract)：
目的建立高效液相色谱法测定富马酸二甲酯原料药中有关物质的方法。方法采用Thermo C18色谱柱,以乙腈-体积分数为0.05%的磷酸溶液(体积比为10∶90)为流动相,流速:1 m L·min-1,检测波长:211 nm,进样量:20μL,柱温:35℃。结果杂质A、B、C、D和富马酸二甲酯的定量限分别为0.009、0.036、0.014、0.073和0.020 mg·L-1,杂质A、B、C、D和富马酸二甲酯的线性分别为0.160~1.602、0.160~1.599、0.160~1.602、0.160~1.600和0.160~1.601 mg·L-1,杂质A、B、C、D的平均回收率分别为98.5%、98.5%、100.0%和98.6%。结论本法可作为富马酸二甲酯有关物质的测定方法。
Objective To develop an HPLC method for the determination of the related substances of dimethyl fumarate. Methods The separation was performed on a C18 column with mobile phase consisted of acetonitrile- 0. 05% phosphoric acid( V ∶ V = 10∶ 90). The detection wavelength was 211 nm and the column temperature was set at 35 ℃. The flowrate was 1 m L·min- 1and the injection volume was 20 μL. Results The limit of quantitation of dimethyl fumarate and its impurities A,B,C and D were 0. 020,0. 009,0. 036,0. 014 and 0. 073 mg·L- 1,respectively. The linear range of dimethyl fumarate and its impurities A,B,C and D were 0. 160-1. 601,0. 160-1. 602,0. 160-1. 599,0. 160-1. 602 and 0. 160-1. 600 mg·L- 1,respectively. The average recoveries of impurities A,B,C and D were 98. 5%,98. 5%,100. 0% and 98. 6%,respectively.Conclusions The established method is simple,accurate,specific and sensitive,which can be used for the quality control of dimethyl fumarate and its related substances.
关键词(KeyWords)：
富马酸二甲酯;有关物质;高效液相色谱法
dimethyl fumarate;related substances;HPLC
基金项目(Foundation):
作者(Author):
于小涵,周现滢,安珍珍,于治国
YU Xiao-han,ZHOU Xian-ying,AN Zhen-zhen,YU Zhi-guo
DOI: 10.14066/j.cnki.cn21-1349/r.2015.11.007
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