Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
46, Number 8, September 2008, pp. 680-685
Ultrasonic assisted SPME Coupled with GC and
GC–MS using Pencil Lead as a Fiber for Monitoring the Organic
Volatile Impurities of Ceftazidime
Djavanshir Djozan1, Abolghasem Jouyban2,
and Jamal Norouzi1 1Department of Analytical Chemistry, Faculty of Chemistry, University
of Tabriz, Tabriz, Iran and 2Faculty of Pharmacy and Drug Applied
Research Center, Tabriz University of Medical Sciences, Tabriz,
Iran
A simple, rapid, non-destructive, and in-situ method for the isolation and sampling of organic volatile impurities
in Ceftazidime is developed using solid-phase microextraction
(SPME). For the monitoring of the extracted compounds, gas chromatography
(GC) and GC–mass spectrometry analyses are used. The effective
factors such as nature of the fiber, SPME mode, extraction temperature,
and ultrasonic assistance have been investigated and detailed
here. Qualification studies reveal the existence of pyridine
(as a degradation product of ceftazidime) and the residual solvents;
acetone, methylene-chloride, and diethylamine are the main impurities
in the studied pharmaceutical. External standard method is used
for quantitative analysis. The % relative standard deviation
values are below 10%, and the limits of detection for the detected
solvents are 1.06, 0.98, 0.83, and 0.51 ppm, respectively. The
proposed method is both accurate and linear and could be used
in quality control of ceftazidime and also its stability investigations.
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