Simultaneous determination of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) enantiomers by GC-MS

Simultaneous determination of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) enantiomers by GC-MS
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DOI:
10.1093/jat/23.6.518
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发表时间:
1999-10-01
影响因子:
2.5
通讯作者:
Cody, JT
Cody, JT
中科院分区:
医学3区
文献类型:
--
作者:
Hensley, D;Cody, JT

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建立了同时测定尿中苯丙胺、甲基苯丙胺、3,4-亚甲基二氧基苯丙胺(MDA)、3,4-亚甲二氧基甲基苯丙胺(MDMA)和3,4-亚甲二氧乙基苯丙胺(MDEA)对映体比例的方法。方法采用液-液萃取,三氟乙酰-L-丙酰氯(L-TPC)衍生化,气相色谱-质谱法分析。该分析是使用制备的样品开发的,该样品包含在每个对映体的百分比范围内的每个分析物的不同浓度。结果表明,对于≥含量为10 ng/mL苯丙胺和甲基苯丙胺,以及≥含量为25 ng/mL丙二醛、甲基二乙醇胺和甲基二乙醇胺的样品,该方法可以提供准确可靠的结果。该分析方法用于分析MDMA对照研究对象的尿样。结果8名受试者最初均显示MDMA的l-对映体所占比例较大,且随着给药时间的延长而增加。对代谢产物丙二醛的分析表明,d-对映体的比例最初大于l-对映体的比例,然后l-对映体的比例逐渐增加,直到超过l-对映体的量。在所有病例中,l-丙二醛在给药后36小时内都超过了hED-丙二醛。
A method is described for the simultaneous determination of the ratio ofl- andd-enantiomers of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) in urine. The assay uses liquid-liquid extraction followed by derivatization with trifluoroacetyl-l-prolyl chloride (l-TPC) and analysis by gas chromatography-mass spectrometry. The assay was developed using prepared samples containing varying concentrations of each of the analytes over a range of percentages of each enantiomer. Results showed the method to provide accurate and reliable results in samples containing ≥ 10 ng/mL amphetamine and methamphetamine and ≥ 25 ng/mL MDA, MDMA, and MDEA. The assay was used to analyze urine samples from subjects of a controlled MDMA study. Results for each of the eight subjects showed a greater percentage of thel-enantiomer of MDMA initially, and the percentage increased with time postdose. Analysis of the metabolite MDA revealed that the proportion ofd-enantiomer was initially greater than thel-enantiomer followed by a gradual increase in the proportion ofl-enantiomer until it exceeded the amount of thel-enantiomer. In all cases, thel-MDA exceeded thed-MDA within the first 36 h postdose.