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使用整体硅胶盘填充旋转柱和高效液相色谱 - 二极管阵列检测法从尿液中提取苯丙胺类和亚甲二氧基苯丙胺类物质。

Extraction of amphetamines and methylenedioxyamphetamines from urine using a monolithic silica disk-packed spin column and high-performance liquid chromatography-diode array detection.

作者信息

Namera Akira, Nakamoto Akihiro, Nishida Manami, Saito Takeshi, Kishiyama Izumi, Miyazaki Shota, Yahata Midori, Yashiki Mikio, Nagao Masataka

机构信息

Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kaumi 1-2-3, Minami-ku, Hiroshima 734-8551, Japan.

出版信息

J Chromatogr A. 2008 Oct 24;1208(1-2):71-5. doi: 10.1016/j.chroma.2008.08.091. Epub 2008 Sep 2.

DOI:10.1016/j.chroma.2008.08.091
PMID:18790482
Abstract

To overcome the limitations of solid-phase extraction, we developed a device comprising a spin column packed with octadecyl silane-bonded monolithic silica for extracting amphetamines and methylenedioxyamphetamines from urine. Urine (0.5mL), buffer (0.4mL), and methoxyphenamine (internal standard) were directly put into the preactivated column. The column was centrifuged (3000rpm, 5min) for sample loading and washed. The adsorbed analytes were eluted and analyzed by high-performance liquid chromatography, without evaporation. The results were as follows: linear curves (drug concentrations of 0.2-20microg/mL); correlation coefficients >0.99; detection limit, 0.1microg/mL. The proposed method is not only useful for drugs from biological materials but also highly reproducible for the analysis of these drugs in urine.

摘要

为克服固相萃取的局限性,我们开发了一种装置,该装置包括一个填充有十八烷基硅烷键合整体硅胶的旋转柱,用于从尿液中提取苯丙胺类和亚甲二氧基苯丙胺类物质。将尿液(0.5mL)、缓冲液(0.4mL)和甲氧苯丙胺(内标)直接加入预活化的柱中。将柱离心(3000转/分钟,5分钟)以进行样品加载和洗涤。吸附的分析物经洗脱后通过高效液相色谱法进行分析,无需蒸发。结果如下:线性曲线(药物浓度为0.2 - 20微克/毫升);相关系数>0.99;检测限为0.1微克/毫升。所提出的方法不仅对生物材料中的药物有用,而且对尿液中这些药物的分析具有高度重现性。

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