Determination of residual organic solvents in Apixaban bulks drug by headspace gas chromatography
10.7501/j.issn.1674-6376.2017.01.011
- VernacularTitle:顶空气相色谱法测定阿哌沙班原料药中有机溶剂残留
- Author:
Dongfang LIU
;
Xiucai GUO
;
Lina ZHAO
;
Chaodong JIN
- Keywords:
Apixaban;
headspace gas chromatography;
residual organic solvents
- From:
Drug Evaluation Research
2017;40(1):63-67
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a method for determination of the twelve residual organic solvents,including methanol,ethanol,acetone,isopropanol,tert-Butyl methyl ether,dichloromethane,aceticether,tetrahydrofuran,triethylamine,trimethylorthofor-Mate,morpholine,N,N-Dimethylformamide in Apixaban bulks drug.Methods Gas head-space chromatography was applied to this study.The column was DB-624 silica capillary column (30.0 m × 0.53 mm × 3.00 μm) and the carrier gas was high purity nitrogen;The vial temperature was 100 ℃,and the vial time was 20 min.The Column temperature was kept at 40 ℃ for 6 min,then the temperature was raised to 220 ℃ at the rate of 20 ℃/min and subsequently sustained for 10 min.FID detector temperature and injection temperature were both 250 ℃.The N2 flow rate was 2.8 mL/min.Split ratio was 5∶1.Results Twelve kinds of solvents were completely separated and determined with a good linearity (r =0.9994-0.9999).The RSD values of precision experiments and the average recovery was in line with the requirements.Conclusion Theanalytical method is simple,accurate and sensitive,which could be used for determination of residual organic solvents in Apixaban bulks drug.
