Determination of Two Kinds of Residual Solvents in Flurbiprofen Axetil by Capillary Gas Chromatography
10.6039/j.issn.1001-0408.2016.21.35
- VernacularTitle:毛细管GC法测定氟比洛芬酯原料药中两种溶剂残留量
- Author:
Yuncheng GUO
;
Xue LI
;
Ling ZHONG
- Publication Type:Journal Article
- Keywords:
Flurbiprofen axetil;
Capillary gas chromatography;
1,1-ethanediol diacetate;
Acetic acid;
Residual
- From:
China Pharmacy
2016;27(21):2988-2989,2990
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil. METHODS:Capillary gas chromatography was performed on the column of DB-FFAP capillary column by temperature pro-grammed,the inlet temperature was 150 ℃,flame ionization detector was chosen,detector temperature was 290 ℃,carrier gas was nitrogen at a flow rate of 1.0 ml/min,injection volume was 1.0 μl,and split ratio was 5∶1. RESULTS:1,1-ethanediol diacetate and acetic acid were well-separated;and the linear ranges was 0.78-19.55 g/ml(r=0.999 7)and 7.69-64.11 μg/ml(r=0.999 3),re-spectively;the limits of quantification were 0.78 μg/ml and 7.69 μg/ml,and limits of detection were 0.23 μg/ml and 2.56 μg/ml for 1,1-ethanediol diacetate and acetic acid respectively;RSDs of precision and reprocudibility tests were lower than 3%,and stability test was lower than 5%;recoveries were 97.6%-100.4%(RSD=0.94%,n=9)and 93.6%-100.4%(RSD=0.94%,n=9);and the test results for 3 batches of flurbiprofen axetil were met the specification. CONCLUSIONS:The method is simple,accurate and re-liable,and can be used for the determination of 1,1-ethanediol diacetate and acetic acid in flurbiprofen axetil.
