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顶空进样气相色谱法测定瑞替加滨中溶剂残留
引用本文:高海鹰,孟黎明,王海玲,关悦. 顶空进样气相色谱法测定瑞替加滨中溶剂残留[J]. 化学分析计量, 2017, 26(1). DOI: 10.3969/j.issn.1008-6145.2017.01.003
作者姓名:高海鹰  孟黎明  王海玲  关悦
作者单位:吉林省药物研究院,长春,130061
基金项目:吉林省科技发展计划项目
摘    要:建立瑞替加滨原料药中甲醇、异丙醇、乙酸乙酯残留溶剂的测定方法。以二甲基亚砜(DMSO)为溶剂,DB–WAX123–7032石英毛细管柱为色谱分离柱,FID检测器,程序升温,氮气为载气。甲醇、异丙醇、乙酸乙酯能得到良好分离,甲醇在29.23~292.30μg/m L范围内有良好的线性,线性相关系数为0.996,平均回收率为103.83%;异丙醇在49.96~499.60μg/m L范围内有良好的线性,线性相关系数r=0.996,平均回收率为105.16%;乙酸乙酯在51.59~515.90μg/m L范围内有良好的线性,线性相关系数为0.996,平均回收率为101.36%。甲醇、异丙醇、乙酸乙酯的检出限分别为0.036,0.213,0.062μg/m L,测定结果的相对标准偏差分别为4.96%,4.52%,4.34%(n=6)。该方法灵敏度高,可用于瑞替加滨原料药中有机溶剂的检测。

关 键 词:顶空进样气相色谱法  瑞替加滨  甲醇  异丙醇  乙酸乙酯

Determination of Residual Solvents in Retigabine by Headspace Capillary Gas Chromatography
Gao haiying,Meng Liming,Wang Hailing,Guan Yue. Determination of Residual Solvents in Retigabine by Headspace Capillary Gas Chromatography[J]. Chemical Analysis And Meterage, 2017, 26(1). DOI: 10.3969/j.issn.1008-6145.2017.01.003
Authors:Gao haiying  Meng Liming  Wang Hailing  Guan Yue
Abstract:A method for determining methanol,isopropanol and ethyl acetate in retigabine material by headspace gas chromatography was established.The solvent media was dimethyl sulfoxide(DMSO),the seperation was carried on DBWAX123-7032 capillary column with the FID detector at temperature programming,the carrier gas was nitrogen.The result showed that the three solvents were completely separated.The standard curve of methanol was linear in the range of 29.23-292.30 μ g/mL,r=0.996,the average recovery was 103.83%.The standard curve of isopropanol was linear in the range of 49.96-499.60 μg/mL,r=0.996,the average recovery was 105.16%.The standard curve of ethyl acetate was linear in the range of 51.59-515.90 μ g/mL,r=0.996,the average recovery was 101.36%.The detector limit of methanol,isopropanol and ethyl acetate were 0.036,0.213 and 0.062 μ g/mL,and the relative standard deviations of detection results were 4.96%,4.52%,4.34%(n=6),repectively.The method is sensitive and it can be used for the detection of three residual solvents in retigabine.
Keywords:headspace gas chromatography  retigabine  methanol  isopropanol  ethyl acetate
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