科研之友
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摘要
A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid-phase microextraction with gas chromatography-flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5ml of aqueous solution with pH 10.0 into an organic extracting solvent (1-octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 mu l of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1-octanol as extracting solvent, stirring rate of 700rpm, 15% (w/v) salt addition, pH 10.0 and 25min sampling time at 50 degrees C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500ng/ml for sufentanil and 0.1 to 500ng/ml for alfentanil. Limits of detection 0.01 and 0.02ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra-day and inter-day standard deviations were found to be less than 8.4% (n=5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples.
- 出版日期2013-7
