Determination of Five Residual Solvents in Vidarabine Monophosphate by Headspace Gas Chromatography
10.6039/j.issn.1001-0408.2016.24.29
- VernacularTitle:顶空气相色谱法测定单磷酸阿糖腺苷原料药中5种残留溶剂
- Author:
Xuwen JIAO
;
Hua CHEN
;
Weiyang LIANG
- Publication Type:Journal Article
- Keywords:
Vidarabine monophosphate;
Headspace GC;
Residual solvent;
Determination
- From:
China Pharmacy
2016;27(24):3408-3409,3410
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for the determination of ethanol,acetonitrile,dichloromethane,ethyl acetate, pyridine in vidarabine monophosphate. METHODS:Headspace GC was performed on the column of Agilent DB-624,programmed temperature,inlet temperature was 200 ℃,the detector was flame ionization detector,detecting temperature was 250 ℃,nitrogen was carrier gas,flow rate was 3 ml/min,split ratio was 1∶1,the top bottles equilibrium temperature was 100 ℃,and equilibrium time was 45 min,injection volume was 1 ml. external standard was used for quantitative analysis. RESULTS:The peaks of five re-sidual solvents could be completely separated from the other peaks respectively,The linear rang was 24.7-296.3 μg/ml for ethanol (r=0.999 6)、1.9-23.2 μg/ml for acetonitrile(r=0.999 0),2.8-33.6 μg/ml for dichloromethane(r=0.998 0),24.7-295.9 μg/ml for ethyl acetate(r=0.999 5),1.0-11.9 μg/ml for pyridine(r=0.998 6);RSDs of precision and reproducibility tests were lower than 4.35%;recoveries were 102.4%(RSD=2.0%,n=9)、102.1%(RSD=3.4%,n=9)、105.5%(RSD=4.8%,n=9)、100.3%(RSD=4.8%, n=9)、98.3%(RSD=4.0%,n=9). The minimum quantifation limit was 0.304 4-0.988 0 μg/ml and the minimum detection limit was 0.101 5-0.329 3 μg/ml. CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for the determination of residual solvents in vidarabine monophosphate.
