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采用分子印迹固相萃取法,通过气相色谱-质谱联用技术,对人体全血中的甲基苯丙胺、苯丙胺和亚甲二氧基苯丙胺等苯丙胺类兴奋剂进行选择性测定。

Molecularly imprinted solid-phase extraction for the selective determination of methamphetamine, amphetamine, and methylenedioxyphenylalkylamine designer drugs in human whole blood by gas chromatography-mass spectrometry.

机构信息

Department of Legal Medicine, Showa University School of Medicine, Tokyo, Japan.

出版信息

J Sep Sci. 2012 Mar;35(5-6):726-33. doi: 10.1002/jssc.201100924. Epub 2012 Jan 24.

Abstract

A novel method is described for the extraction of methamphetamine, amphetamine, and methylenedioxyphenylalkylamine designer drugs, such as 3,4-methylenedioxy-methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxyethylamphetamine, N-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine, and 3,4-(methylenedioxyphenyl)-2-butanamine, from human whole blood using molecularly imprinted solid-phase extraction as highly selective sample clean-up technique. Whole blood samples were diluted with 10 mmol/L ammonium acetate (pH 8.6) and applied to a SupelMIP-Amphetamine molecularly imprinted solid-phase extraction cartridge. The cartridge was then washed to eliminate interferences, and the amphetamines of interest were eluted with formic acid/methanol (1:100, v/v). After derivatization with trifluoroacetic anhydride, the analytes were quantified using gas chromatography-mass spectrometry. Recoveries of the seven amphetamines spiked into whole blood were 89.1-102%. The limits of quantification for each compound in 200 μL of whole blood were between 0.25 and 1.0 ng. The maximum intra- and inter-day coefficients of variation were 9.96 and 13.8%, respectively. The results show that methamphetamine, amphetamine, and methylenedioxyphenylalkyl-amine designer drugs can be efficiently extracted from crude biological samples such as whole blood by molecularly imprinted solid-phase extraction with good reproducibility. This extraction method will be useful for the pretreatment of human samples before gas chromatography-mass spectrometry.

摘要

描述了一种从全血中提取甲基苯丙胺、苯丙胺和亚甲二氧基苯丙胺类设计药物(如 3,4-亚甲二氧基甲基苯丙胺、3,4-亚甲二氧基苯丙胺、3,4-亚甲二氧基乙基苯丙胺、N-甲基-1-(3,4-亚甲二氧基苯基)-2-丁胺和 3,4-(亚甲二氧基苯基)-2-丁胺)的新方法,该方法使用分子印迹固相萃取作为高度选择性的样品净化技术。将全血样品用 10 mmol/L 乙酸铵(pH 8.6)稀释,然后应用于 SupelMIP-苯丙胺分子印迹固相萃取柱。然后用洗脱液冲洗萃取柱以去除干扰物,并用甲酸/甲醇(1:100,v/v)洗脱目标苯丙胺。用三氟乙酸酐衍生化后,使用气相色谱-质谱法定量分析。七种苯丙胺类化合物在全血中的加标回收率为 89.1-102%。在 200 μL 全血中,每种化合物的定量限在 0.25-1.0 ng 之间。日内和日间变异系数的最大值分别为 9.96%和 13.8%。结果表明,通过分子印迹固相萃取可以从全血等粗生物样品中高效提取甲基苯丙胺、苯丙胺和亚甲二氧基苯丙胺类设计药物,且重现性良好。这种提取方法将有助于在气相色谱-质谱分析前对人体样本进行预处理。

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