Determination of 6 residual solvents in selexipag by headspace gas chroma-tography
10.11665/j.issn.1000 -5048.20180113
- VernacularTitle:顶空气相色谱法测定selexipag中6种有机溶剂残留量
- Author:
Lili LI
1
;
Hongpeng WANG
;
Haiwei TIAN
;
Jin LI
;
Shuangshuang GAO
;
Jing HA
Author Information
1. 河北科技大学化学与制药工程学院
- Keywords:
selexipag;
headspace gas chromatography;
residual solvents
- From:
Journal of China Pharmaceutical University
2018;49(1):93-96
- CountryChina
- Language:Chinese
-
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.
