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首页> 外文期刊>Rapid Communications in Mass Spectrometry: RCM >Determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, and 3,4-methylenedioxymethamphetamine in urine by online solid-phase extraction and ion-pairing liquid chromatography with detection by
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Determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, and 3,4-methylenedioxymethamphetamine in urine by online solid-phase extraction and ion-pairing liquid chromatography with detection by

机译:在线固相萃取-离子对液相色谱法测定尿中的苯丙胺,甲基苯丙胺,3,4-亚甲基二氧基苯丙胺,3,4-亚甲基二氧基乙基苯丙胺和3,4-亚甲基二氧基甲基苯丙胺

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摘要

A method using an online solid-phase extraction (SPE) and ion-pairing liquid chromatography with electrospray tandem mass spectrometry (LC/ES-MS/MS) was developed for determination of amphetamine (Amp), methamphetamine (mAmp), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA), and 3,4-methylenedioxymethamphetamine (MDMA) in urine samples. A SPE cartridge column with both hydrophilic and lipophilic functions was utilized for online extraction. A reversed-phase C-18 LC column was employed for LC separation and MS/MS was used for detection. Trifluoroacetic acid was added to the mobile phase as an ion-pairing reagent. This method was fully automated and the extraction and analysis procedures were controlled by a six-port switch valve. Recoveries ranging from 85-101% were measured. Good linear ranges (10-500 ng/mL) for Amp and mAmp were determined. For MDA, MDMA and MDEA, dual linear ranges were obtained from 5-100 and 100-500 ng/mL, respectively. The detection limit of each analytical compound, based on a signal-to-noise ratio of 3, ranged from 1-3 ng/mL. The applicability of this newly developed method was examined by analyzing several urine samples from drug users. Good agreement was obtained between the results from this method and a literature GC/MS method. Copyright (c) 2005 John Wiley A Sons, Ltd.
机译:建立了一种使用在线固相萃取(SPE)和离子对液相色谱与电喷雾串联质谱(LC / ES-MS / MS)的方法来测定苯丙胺(Amp),甲基苯丙胺(mAmp),3,4尿液样本中的-亚甲二氧基苯丙胺(MDA),3,4-亚甲二氧基乙基苯丙胺(MDEA)和3,4-亚甲二氧基甲基苯丙胺(MDMA)。具有亲水和亲脂功能的SPE柱可用于在线提取。使用反相C-18 LC色谱柱进行LC分离,并使用MS / MS进行检测。将三氟乙酸作为离子对试剂添加到流动相中。该方法是全自动的,提取和分析程序由六通切换阀控制。测定的回收率为85-101%。确定了Amp和mAmp的良好线性范围(10-500 ng / mL)。对于MDA,MDMA和MDEA,双线性范围分别从5-100 ng / mL和100-500 ng / mL获得。基于3的信噪比,每种分析化合物的检出限为1-3 ng / mL。通过分析一些吸毒者的尿液样本,检查了这种新开发方法的适用性。此方法的结果与文献GC / MS方法之间取得了很好的一致性。版权所有(c)2005 John Wiley A Sons,Ltd.

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