Extraction of amphetamines and methylenedioxyamphetamines from urine using a monolithic silica disk-packed spin column and high-performance liquid chromatography-diode array detection.
Extraction of amphetamines and methylenedioxyamphetamines from urine using a monolithic silica disk-packed spin column and high-performance liquid chromatography-diode array detection.
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DOI：
10.1016/j.chroma.2008.08.091
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发表时间：
2008-10
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通讯作者：
A. Namera;Akihiro Nakamoto;Manami Nishida;Takeshi Saito;Izumi Kishiyama;S. Miyazaki;M. Yahata;M. Yashiki;Masataka Nagao
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文献类型：
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作者：
A. Namera;Akihiro Nakamoto;Manami Nishida;Takeshi Saito;Izumi Kishiyama;S. Miyazaki;M. Yahata;M. Yashiki;Masataka Nagao
为了克服固相萃取的局限性，我们开发了一种包括填充十八烷基硅烷键合整体硅胶的旋转柱的装置，用于从尿液中提取苯丙胺和亚甲二氧基苯丙胺。尿液(0.5ml)、缓冲液(0.4ml)和甲氧苯那明(内标)直接进入预活化色谱柱。将色谱柱离心(3000转/分，5分钟)以装载样品并洗涤。被吸附的分析物被洗脱并用高效液相色谱分析，不需要蒸发。结果表明：线性关系良好(药物浓度在0.2~20μg/mL范围内)，相关系数r=0.99，检出限为0.1μg/mL。该方法不仅适用于生物原料中的药物，而且对尿液中这些药物的分析具有很高的重复性。
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 0.2–20μg/mL); correlation coefficients >0.99; detection limit, 0.1μg/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.