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Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography
Author(s) -
Frost Richard P.,
Hussain Mumtaz S.,
Raghani Anil R.
Publication year - 2003
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301528
Subject(s) - chemistry , chromatography , gas chromatography , extraction (chemistry) , solid phase microextraction , analyte , adsorption , flame ionization detector , fiber , detection limit , impurity , amine gas treating , divinylbenzene , analytical chemistry (journal) , solid phase extraction , gas chromatography–mass spectrometry , mass spectrometry , organic chemistry , styrene , copolymer , polymer
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.