Application Of Hollow Fiber Liquid Phase Microextraction For The Determination Of Three Analgesic And Narcotic Drugs In Water And Biological Fluid

Application of hol low fiber Iiquid phase microextraction for the determination of three analgesic and narcotic drugs in water and biological fluidIntroductionHollow fiber liquid-phase microextraction(HF-LMPE) is a novel method sample preparation in recent years. It is a miniaturized implementation of conventional liquid-liquid extraction(LLE). Normally, this technique is carded out by using a porous hollow fiber membrane as interface between the sample(aqueous solution) and organic solvent, which avoiding mixing of the two phases. The present study HF-LPME has been applied to the extraction of pethidine, ketamine and tramadol from water and biological fluid.ExperimentalMethod parameters were optimized and experimental conditions were: pH 11.5, containing saturated NaC1, stirred at 600rpm, extracted with toluene for 20min, nefopame hydrochloride as internal standard. A 4.0μ1 aliquot of toluene was withdrawn into the 5μ1 syringe and injected into polyvinylidene fluoride(PVDF) hollow fiber membrane. After 20min the analyte-enriched was withdrawn into the syringe and injected into the heated injection port of the GC-FID for further analysis. The injector was operating at 250℃in the splitless and detector temperature was 260℃. Nitrogen was used as the carder gas at a flow-rate of 10-11ml/min. The column oven was initially set at 100℃for 1min, programmed to 280℃at a 30℃/min rate. In these conditions, the four compounds were separated very well. The linearity, precision, limits of detection(LODs) and relative recovery of pethidine, ketamine and tramadol in water, urine and plasma were calculated respectively.ResultsCorrelation coefficients: pethidine were 0.9935(plasma),0.9981(urine) and 0.9997(water), ketamine were 0.9906(urine), 0.9913(plasma) and 0.9927(water), tramadol were 0.9741(urine), 0.9913(water) and 0.9970(plasma); LODs: pethidine,ketamine and tramadol were 0.01μg/ml in water and urine and 0.05μg/ml in plasma respectively; RSDs for intra-day: pethidine were 4.6%(water),7.3%(urine) and 13.0%(plasma), ketamine were 1.4% (water), 13.6%(urine) and 15.1%(plasma), tramadol were 3.7%(plasma),4.3%(urine) and 9.0%(water); RSDs for inter-day: pethidine were 12.2%(water),13.5 %(urine) and 15.1%(plasma), ketamine were 5.3%(urine), 6.0%(water) and 12.3%(plasma), tramadol were 7.1%(plasma),11.9%(water) and 15.5%(urine); Relative recoveries: pethidine were 93.49%(urine),97.57%(water) and 109.80%(plasma), ketamine were 91.09%(plasma),100.40%(water) and 101.80%(urine), tramadol were 92.94%(urine), 106.40%(plasma) and 113.32%(water).ConelusionThe results demonstrated good selectivity, linearity and acceptable limits of detection and repeatibility. Determination of pethidine, ketamine hydrochloride, tramadol hydrochloride from water and biological fluid using hollow fiber liquid phase microextraction was simple, efficient, practical and requiring little solvent, avoiding carry-over and cross pollution. HF-LPME integrated extraction, concentration and sample introduction in one step simultaneously. Thus we can improve the speed of sample analysis. HF-LPME was evolution to traditional LLE. It has a better foreground in extraction of organic compounds from water and a large application in pharmaceutical analysis, drug analysis and analysis of trace insecticide in water and soil etc.