微乳液毛细管电动色谱-场放大富集法灵敏分析尿液中的9种麻醉剂类药物

建立了一种微乳液毛细管电动色谱（MEEKC）-场放大富集（FASI）分析尿液中多种麻醉剂（吗啡、可待因、纳洛酮、海洛因、蒂巴因、可卡因、哌替啶、芬太尼、美沙酮）的方法。考察了微乳液组成、分离电压等因素的影响，得到的最佳微乳液组成（质量分数）为0. 6% 十二烷基硫酸钠、1.2% 正丁醇、0.6% 乙酸乙酯和 97.6% 10 mmol/L 硼砂缓冲液（pH 9.5）；分离电压为25 kV。在上述微乳体系中，9种化合物在 15 min 内得到了基线分离。采用场放大在线富集技术提高了分析灵敏度，检出限 (S/N = 3) 低至 0.3 µg/L。模拟尿样样品中9种麻醉剂的加标回收率介于79.4% ~ 119.9% 之间，日内相对标准偏差小于  5.5%。将该方法应用于美沙酮大鼠体外代谢样品的测定，结果令人满意。

A simple,sensitive and reproducible method using microemulsion electrokineticchromatography (MEEKC) -field amplified sample injection (FASI) was developedfor the anal­ysis of nine narcotics (morphine, codeine, naloxone, heroin,thebaine, cocaine, pethidine, fentanyl and methadone) in urine. In the MEEKCmethod, sodium dodecyl sulfate (SDS) , 1 -butanol and ethyl acetate were usedas surfactant, co-surfactant and organic solvent, respec­tively. The effects ofthe acidity and concentration of borate buffer, SDS, 1 -butanol and ethylacetate contents were investigated. The optimum concentrations (by massfraction) of microemulsion system were 0.6% SDS, 1.2% 1-butanol, 0.6% ethyl acetate and 97. 6% 10 mmol/L Na₂ B₄ O₇buffer (pH 9.5). The applied voltage was 25 kV. FASI was coupled with the MEEKCmethod to increase the sensitivity. Under the optimum conditions, the ninenarcotics were baseline separated within 15 min and the detection limits (S/N= 3) were in the range of 0.3 - 8.0 µg/L. The spiked recoveries in urinesamples were between 79.4% and 119.9% with the intradayrelative standard deviations (RSDs) less than 5.5%. The developed method hasbeen successfully applied to the analysis of methadone in the samples from invitro metabolism study.