Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography
Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography
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DOI：
10.1016/j.chroma.2012.05.085
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发表时间：
2012-07-27
影响因子：
4.1
通讯作者：
Baheri, Tahmineh
中科院分区：
文献类型：
--
作者：
Djozan, Djavanshir;Farajzadeh, Mir Ali;Baheri, Tahmineh
在这项研究中，报告了一种利用分子印迹固相萃取（MISPE）以及同时衍生化和分散液液微萃取（DLLME）从尿液样品中提取和预浓缩甲基苯丙胺（MAMP）和3,4-亚甲基二氧基甲基苯丙胺（MDMA，摇头丸）的先进技术。以MAMP为模板，采用沉淀聚合法制备了固相萃取（SPE）分子印迹微球吸附剂。目标分析物的水溶液通过MAMP-MIP墨盒，然后用甲醇洗脱吸附的分析物。收集的洗脱液与氯甲酸丁酯混合，作为衍生试剂和萃取溶剂。将混合物立即注入去离子水中。离心后，将沉淀的有机相1 μ L注入气相色谱-火焰离子化检测（GC-FID）或气相色谱-质谱联用（GC-MS）。对影响这两个步骤（MISPE和DLLME）性能的各种实验参数进行了深入研究。校准图在10 ~ 1500 ng mL(-1) （MAMP）和50 ~ 1500 ng mL(-1) （MDMA）范围内呈线性关系，检出限（lod）分别为2和18 ng mL（-1）。6次重复实验（每种药物100 ng mL(-1)）所得的相对标准偏差（% rsd）分别为5.1%和6.8%。在加标不同浓度的药物的情况下，分析物在人尿样品中的相对回收率在80-88%之间。(c) 2012 Elsevier B.V.版权所有
In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1 mu L of the settled organic phase was injected into gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10-1500 ng mL(-1) (MAMP) and 50-1500 ng mL(-1) (MDMA), and the detection limits (LODs) were 2 and 18 ng mL(-1), respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100 ng mL(-1) of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80-88%. (c) 2012 Elsevier B.V. All rights reserved.