Analyzing Trace Levels of Carbon Tetrachloride in a Drug Substance by Headspace GC with Flame Ionization Detection

作者：Natarajan S^*; Kempegowda B K

来源：LC-GC North America, 2015, 33(9): 718-726.

A simple and accurate method for determining trace levels of the carcinogenic solvent carbon tetrachloride (CCl4) in flunixin meglumine, a white crystalline powder drug substance, was developed using gas chromatography (GC). The method was observed to be robust, and complete analytical method validation was performed and met the requirements as per International Conference on Harmonization (ICH) guidelines. The method provides a lower detection level than other currently available methods. The limit of quantification (LOQ) achieved by this method was 0.8 ppm and calibration curves were linear, with R > 0.998. In general, for the analysis of halogenated compounds, electron capture detection (ECD) has mostly been used, and in this proposed method flame ionization detection (FID) with an internal standard was used. The method was implemented successfully for various active pharmaceutical ingredients (APIs).

• 出版日期2015-9