摘要
利用离子液体分散液相微萃取技术,结合高效毛细管电泳技术,对尿液中痕量麻黄碱和氯胺酮毒品实现高效富集及分离检测。实验中,对影响萃取效率的因素,包括离子液体和分散剂的种类及用量、样品溶液中NaOH的加入量、反萃取试剂HCl的加入量等进行了优化。0.5mL预处理过的样品溶液加入3.5mL0.2g/LNaOH溶液,以40mL[BMIM]PF6为萃取溶剂,350mL乙腈为分散剂萃取数秒后,反萃取通过向富含离子液体的上清液中加入60μL0.1mol/LHCl完成。麻黄碱和氯胺酮在0.10～10mg/L范围内具有良好的线性关系（r2分别为0.9968和0.9981）;富集因子分别为28.8和16.9,检出限为0.015和0.03mg/L（S/N=3）;重现性RSD〈6.8%（n=6）。本方法成功应用于尿液中麻黄碱和氯胺酮的分析检测,检出限分别为0.21和0.39mg/L,加标回收率为79%～90%。本方法具有价廉、易操作、高富集、检测灵敏及干扰小等特点,可用于生物检材中痕量毒品的检测。
A method for dispersive liquid-liquid microextraction using ionic-liquid was applied for preconcentration, separation and simultaneous detection of trace-amount ephedrine and ketamine drugs in urine samples, by coupling with high performance capillary electrophoresis. Various experimental conditions, including selection of ionic-liquid and dispersant and their concentrations, the amount of addition of NaOH and HC1 in the sample, were investigated and optimized. The pretreated sample （0.5 mL） was added into 3.5 mL 0.2 g/L NaOH solution and its extraction was performed within several seconds by using 40 mL [ BMIM ] PF6 as extraction solvent and 350 mL aeetonitrile as dispersant, then the analytes were back-extracted into 60 txL O. 1 mol/L HC1 solution. Under the optimum conditions, the method shows good linearity for detection of ephedrine and ketamine in the range of 0. 10 - 10 mg/L （ r2 is 0. 9968 for ephedrine and 0. 9981 for ketamine）. The enrichment factors for ephedrine and ketamine were achieved to be 28. 8 and 16. 9, respectively, and the LODs were determined to be 0. 015 and 0.03 rag/L, respectively （S/N = 3 ）. The method show good repeatability with RSD less than 6. 8% （n = 6 ）. The feasibility of the method was demonstrated by successful determination of ephedrine and ketamine drugs in urine samples, with spiked recoveries in the range of 79% -90% and LODs （ S/N = 3 ） of 0.21 mg/L for ephedrine and 0.39 mg/L for ketamine. The method has properties such as cheap, easy-to-operate, high enrichment, sensitive detection and little interference, and would have potential application in detection of trace-amount drugs in the biological samples.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2013年第12期1919-1922,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.21175018)
吉林省科技发展基金(No.20120431)资助项目
关键词
离子液体
分散液相微萃取
毛细管电泳
毒品
Ionic liquid
Dispersive liquid-liquid microextraetion
Capillary electrophoresis
Drug of abuse
