色谱

色谱

• 研究论文 • 上一篇    下一篇

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

张雨1, 李琴2, 卢明华3, 张兰2, 陈国南2, 蔡宗苇2,3*   

  1. 1. 中国中医科学院望京医院, 北京 100102; 2. 福州大学, 食品安全分析与检测教育部重点实验室, 福建 福州 350002; 3. 香港浸会大学化学系, 香港九龙塘
  • 收稿日期:2011-06-13 修回日期:2011-06-26 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 蔡宗苇,教授,博士生导师. Tel: （852）34117070,
  • 基金资助:

    国家自然科学基金项目(No. 20928005)和福建省自然科学基金项目(No. 2010J05021)

Analysis of nine narcotics in urine by microemulsion electrokinetic chromatography-field amplified sample injection

ZHANG Yu1, LI Qin2, LU Minghua3, ZHANG Lan2, CHEN Guonan2, CAI Zongwei2,3*   

  1. 1. Wangjing Hospital, China Academy of Chinese Medical Sciences, Beijing 100102, China; 2. Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou 350002, China; 3. Department of Chemistry, Hong Kong Baptist University, Kowloon Tong, Hong Kong SAR, China
  • Received:2011-06-13 Revised:2011-06-26 Online:2011-08-28 Published:2011-09-28

PDF

445

被引次数

15

摘要： 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。

关键词: 场放大富集, 麻醉剂, 尿液, 微乳液毛细管电动色谱

Abstract: A simple, sensitive and reproducible method using microemulsion electrokinetic chromatography (MEEKC)-field amplified sample injection (FASI) was developed for the analysis of nine narcotics (morphine, codeine, naloxone, heroin, thebaine, cocaine, pethidine, fentanyl and methadone) in urine. In the MEEKC method, sodium dodecyl sulfate (SDS), 1-butanol and ethyl acetate were used as surfactant, co-surfactant and organic solvent, respectively. The effects of the acidity and concentration of borate buffer, SDS, 1-butanol and ethyl acetate contents were investigated. The optimum concentrations (by mass fraction) of microemulsion system were 0.6% SDS, 1.2% 1-butanol, 0.6% ethyl acetate and 97.6% 10 mmol/L Na2B4O7 buffer (pH 9.5). The applied voltage was 25 kV. FASI was coupled with the MEEKC method to increase the sensitivity. Under the optimum conditions, the nine narcotics 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 urine samples were between 79.4% and 119.9% with the intraday relative standard deviations (RSDs) less than 5.5%. The developed method has been successfully applied to the analysis of methadone in the samples from in vitro metabolism study.

Key words: field amplified sample injection, narcotics, urine, microemulsion electrokinetic chromatography （MEEKC）