摘要
本文建立了2-[1-(4-氯苯基)2-硝基乙基]丙二酸二甲酯的反相高效液相色谱定量分析方法。色谱柱为WAT054275 Waters Symmetry(250 mm×4.6 mm,5μm)不锈钢柱,流动相为甲醇-水(70+30),流速1 mL/min,波长319 nm,柱温40℃。结果显示,2-[1-(4-氯苯基)2-硝基乙基]丙二酸二甲酯峰型良好,样品中的杂质不干扰测定,标准偏差为0.34%,变异系数为0.35%,线性范围较宽,相关系数为0.9997,样品加标回收率为98.6%~100.8%。该方法简便、重复性好、稳定性高、分析快速,可用于巴氯芬的关键中间体2-[1-(4-氯苯基)2-硝基乙基]丙二酸二甲酯含量的测定。
The 2-[1-（4-chloropheny）2-nitro-ethyl] malonate methyl ester is the key intermediate of baclonfen, which was the first GABAB receptor agonist in clinic. The high performance liquid chromatography quantitative analysis method was developed of the intermediate on WAT054275 Waters Symmetry column（250 mm×4.6 mm,5μm）, detected at 319 nm and eluted by mobile phases[methanol-water（70＋30）,1 mL/min], with the column temperature 40 ℃. It showed that the peak of 2-[1-（4-chlorphenyl）2-nitro-ethyl] malonate was good with nointerference of impurities, the standard deviation was 0.34% and the coefficient of variation was 0.35%, linear range was wide, the correlation coefficients was 0.999 7 and the average recovery was between 98.6% ~ 100.8%. The method is simple, sensitive, accurate, which can be used for rapid identification and determination of 2-[1-（4-chloropheny）2-nitro-ethyl] malonate methyl ester.
作者
孔英戈
汪华
张少云
潘萍
Kong Yingge, Wang Hua, Zhang Shaoyun, Pan Ping(Hengyang Food and Drug Inspection and Testing Center, Hengyang 421001, Chin)
出处
《中国资源综合利用》
2018年第1期9-12,共4页
China Resources Comprehensive Utilization
基金
湖南省科技成果项目(项目编号:943Y20120450)
衡阳市农林卫生科研项目(项目编号:2016KYA 049)的阶段性研究成果之一
