中国药科大学学报2018，Vol.49Issue(1)：93-96,4.DOI:10.11665/j.issn.1000 -5048.20180113
顶空气相色谱法测定selexipag中6种有机溶剂残留量
Determination of 6 residual solvents in selexipag by headspace gas chroma-tography
李丽丽 1王洪朋 1田海伟 1李晋 1高双双 1哈婧1
作者信息
- 1. 河北科技大学化学与制药工程学院,石家庄050018
- 折叠
摘要
Abstract
A headspace gas chromatography method was developed for the determination of six residual solvents including methanol, ethanol, acetone, dichloromethane, tetrahydrofuran and toluene residues in selexipag to provide the experimental basis for its quality control.The samples were separated on Kromat PC-624(V)silica capillary column(30.0 m ×0.32 mm,1.8 μm)using temperature programming.The column temperature was kept at 40 ℃ for 5 min initially,and then raised to 180 ℃ at the rate of 20 ℃ /min and subsequently sustained for 5 min.FID detector temperature was 250 ℃ and injection temperature was 200 ℃.The split ratio was 20 : 1. The six residual solvents are separated completely under the given chromatographic conditions with a good linearity (r=0.998 2-1.000);the results of precision,repeatability and stability experiments met the requirement,and the mean recoveries of all solvents were in the range of 96.67％-101.7％.The analytical method is simple,accurate and sensitive,and it can be used for the determination of residual solvents in selexipag.关键词
selexipag/顶空气相色谱/残留溶剂Key words
selexipag/headspace gas chromatography/residual solvents分类
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李丽丽,王洪朋,田海伟,李晋,高双双,哈婧..顶空气相色谱法测定selexipag中6种有机溶剂残留量[J].中国药科大学学报,2018,49(1):93-96,4.
