Determination of Residual of 4 Kinds Organic Solvents in Ecabet Sodium Crude Drug by Capillary GC
10.6039/j.issn.1001-0408.2015.30.39
- VernacularTitle:毛细管气相色谱法测定依卡倍特钠原料药中4种有机溶剂的残留量
- Author:
Xue DI
;
Yanhua LIU
;
Haibo WANG
;
Hui ZHANG
;
Tianmin WANG
- Publication Type:Journal Article
- Keywords:
Capillary GC;
Ecabet sodium;
Crude drug;
Organic solvent;
Residual
- From:
China Pharmacy
2015;(30):4286-4287,4288
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for the determination of residuals of petroleum ether,ethanol,xylene and ace-tic acid in ecabet sodium crude drug. METHODS:Capillary GC was performed on the column of PGE-20M capillary column at the flow rate of 1.7 ml/min,detector was hydrogen flame ionization detector,carrier gas was nitrogen with high purity,column temper-ature was 45 ℃,maintaining 4 min,it increased to 80 ℃ with rate of 10 ℃/min,then increased to 135 ℃ with rate of 30 ℃/min,maintaining 3 min,the injection mode was direct injection,inlet temperature was 250 ℃,and the volume injection was 1.0 μl. RESULTS:The mass concentration was 0.050-1.952 g/L for petroleum ether,0.050-1.941 g/L for ethanol,0.024-0.948 g/L for xy-lene and 0.050-1.947g/L for acetic acid(r=0.999 1-0.999 7);RSDs of precision,stability and reproducibility tests were no more than 1.7%;recoveries were 99.3%-101.0%(RSD=0.7%,n=9),102.3%-103.7%(RSD=0.4%,n=9),101.2%-102.1%(RSD=0.3%,n=9) and 100.3%-102.2%(RSD=0.6%,n=9),respectively. CONCLUSIONS:The method is simple and accurate,and can be used for the control of residual of organic solvents in ecabet sodium crude drug.
