Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography

✍ Scribed by Richard P. Frost; Mumtaz S. Hussain; Anil R. Raghani

• Publisher: John Wiley and Sons
• Year: 2003
• Tongue: English
• Weight: 431 KB
• Volume: 26
• Category: Article
• ISSN: 1615-9306
• DOI: 10.1002/jssc.200301528

✦ Synopsis

Abstract

A methodology for automated headspace solid‐phase microextraction for the trace analysis of pharmaceutical process‐related toxic impurities such as benzyl chloride, triethyl amine, chloroethyl methyl ether, N‐methylmorpholine, and N‐methylpyrrolidinone by gas chromatography and flame ionization detection is reported. Carboxen/polysiloxane/divinylbenzene fiber showed excellent sensitivity towards these analytes compared to direct injection and the highest sensitivity among the commercial SPME fibers evaluated in this study. However, a profound effect of competition for the available adsorption sites was observed on the Carboxen/PDMS/DVB fiber. The effects of extraction parameters such as extraction time, temperature, agitation rate, and headspace volume were studied. The influence of the addition of inorganic salt on the analyte extraction efficiency was also investigated. The sensitivity of method extended to the sub‐ppm level with acceptable precision and accuracy. The linearity of the method covered one order of magnitude. The narrower linear dynamic range is attributed largely to the limited number of adsorption sites on the Carboxen/PDMS/DVB fiber.