چکیده
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The present study describes a microextraction and determination method for analyzing residual
solvents in pharmaceutical products using dynamic headspace–liquid phase microextraction
technique followed by gas chromatography–flame ionization detection. In this method dimethyl
sulfoxide (μL level) placed into a GC liner‐shaped extraction vessel is used as a collection/extraction solvent. Then the liner is exposed to the headspace of a vial containing the sample solution.
The effect of different parameters influencing the microextraction procedure including collection/extraction solvent type and its volume, ionic strength, extraction time, extraction temperature and concentration of NaOH solution used in dissolving the studied pharmaceuticals are
investigated and optimized. Under the optimum extraction conditions, the method showed wide
linear ranges between 0.5 and 5000 mg L−1. The other analytical parameters were obtained in the
following ranges: enrichment factors 240–327, extraction recoveries 72–98% and limits of
detection 0.1–0.8 mg L−1 in solution and 0.6–3.2 μg g−1 in solid. Relative standard deviations
for the extraction of 100 mg L−1 of each analyte were obtained in the ranges of 4–7 and 5–8%
for intra‐day (n = 6) and inter‐day (n = 4) respectively. Finally the target analytes were determined
in different samples such as erythromycin, azithromycin, cefalexin, amoxicillin and co‐amoxiclav
by the proposed method.
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