水和生物体液中3种镇痛麻醉药中空纤维膜液相微萃取

目的研究采用中空纤维膜液相微萃取(hollowfiber liquid phase microextraction,HF-LPME)法提取水和生物体液中的哌替啶,氯胺酮,曲马多。方法样品调节至pH11.5和盐饱和,磁力搅拌器转速为600转/min,内标为盐酸萘福泮,取4μl甲苯,注入到聚偏氟乙烯中空纤维膜中,萃取20min,抽回1μl甲苯进入GC中进行分析。结果血浆、尿、水相关系数R2:哌替啶分别为0.9935、0.9981、0.9997,氯胺酮分别为0.9906、0.9913、0.9927,曲马多分别为0.9741、0.9913、0.9970;检测限:水、尿中哌替啶、氯胺酮、曲马多均为0.01μg/ml,血浆中哌替啶、氯胺酮、曲马多均为0.05μg/ml;血浆、尿、水日内RSD:哌替啶分别为13.0%、7.3%、4.6%,氯胺酮分别为15.1%、13.6%、1.4%,曲马多分别为3.7%、4.3%、9.0%;血浆、尿、水日间RSD:哌替啶分别为15.1%、13.5%、12.2%,氯胺酮分别为12.3%、5.3%、6.0%,曲马多分别为7.1%、15.5%、11.9%;血浆、尿、水相对回收率:哌替啶分别为109.80%、93.49%、97.57%,氯胺酮分别为91.09%、101.80%、100.40%,曲马多分别为106.40%、92.94%、113.32%。结论中空纤维膜液相微萃取用于水和生物体液中的哌替啶,氯胺酮,曲马多的分析,所需有机溶剂少,避免残留和交叉污染,集萃取,富集,进样于一步完成,简单,高效,实用。

Application of hollow fiber liquid phase microextraction for the determination of three analgesic and narcotic drugs in water and biological fluid

Objective !To develop hollow fiber liquid phase microextraction(HF-LPME) method to extract pethidine,ketamine and tramadol from water and biological fluid.Methods The sample was alkalized at pH 11.5 and saturated with sodium chloride,stirred at 600rpm,nefopam hydrochloride as internal standard,extracted with 4μl toluene in PVDF hollow fiber membrane for 20 minutes.Results Correlation 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).Conclusion 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.