Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
Talanta. 2010 Aug 15;82(3):969-75. doi: 10.1016/j.talanta.2010.06.001. Epub 2010 Jun 8.
A method of hollow fiber (HF) liquid phase microextraction (LPME) combined with gas chromatography (GC)-flame ionization detection (FID) was developed for the simultaneous quantification of trace amphetamine (AP), methamphetamine (MA), methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), caffeine and ketamine (KT) in drug abuser urine samples. The factors affecting on the extraction of six target analytes by HF-LPME were investigated and optimized, and the subsequent analytical performance evaluation and real sample analysis were performed by the extraction of six target analytes in sample solution containing 30% NaCl (pH 12.5) for 20 min with extraction temperature of 30 degrees C and stirring rate of 1000 rpm. Under such optimal conditions, the limits of detection (LODs, S/N=3) for the six target analytes were ranged from 8 microg/L (AP, KT) to 82 microg/L (MDA), with the enrichment factors (EFs) of 5-227 folds, and the relative standard deviations (RSDs, n=7) were in the range of 6.9-14.1%. The correlation coefficients of the calibration for the six target analytes over the dynamic linear range were higher than 0.9958. The application feasibility of HF-LPME-GC-FID in illegal drug monitoring was demonstrated by analyzing drug abuser urine samples, and the recoveries of target drugs for the spiked sample ranging from 75.2% to 119.3% indicated an excellent anti-interference capability of the developed method. The proposed method is simple, effective, sensitive and low-cost, and provides a much more accurate and sensitive detection platform over the conventional analytical techniques (such as immunological assay) for drug abuse analysis.
建立了一种中空纤维(HF)液相微萃取(LPME)与气相色谱(GC)-火焰离子化检测(FID)联用的方法,用于同时定量检测吸毒者尿液样品中的痕量苯丙胺(AP)、甲基苯丙胺(MA)、亚甲二氧基苯丙胺(MDA)、亚甲二氧基甲基苯丙胺(MDMA)、咖啡因和氯胺酮(KT)。考察并优化了影响 HF-LPME 萃取六种目标分析物的因素,并通过在 30%NaCl(pH 12.5)样品溶液中萃取 20 分钟,萃取温度为 30°C,搅拌速度为 1000rpm,对六种目标分析物的萃取进行了后续的分析性能评价和实际样品分析。在最佳条件下,六种目标分析物的检出限(LODs,S/N=3)范围为 8μg/L(AP、KT)至 82μg/L(MDA),富集因子(EF)为 5-227 倍,相对标准偏差(RSD,n=7)为 6.9%-14.1%。六种目标分析物的校准动态线性范围内的相关系数均高于 0.9958。通过分析吸毒者尿液样品,证明了 HF-LPME-GC-FID 在非法药物监测中的应用可行性,加标样品中目标药物的回收率为 75.2%-119.3%,表明该方法具有良好的抗干扰能力。该方法简单、有效、灵敏、成本低,为药物滥用分析提供了比传统分析技术(如免疫测定)更准确、更灵敏的检测平台。