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高效液相色谱法测定生物体液中的美拉胂醇并通过核磁共振光谱法表征两种立体异构体

Determination of melarsoprol in biological fluids by high-performance liquid chromatography and characterisation of two stereoisomers by nuclear magnetic resonance spectroscopy.

作者信息

Ericsson O, Schweda E K, Bronner U, Rombo L, Fridén M, Gustafsson L L

机构信息

Hospital Pharmacy, Huddinge University Hospital, Sweden.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):243-51. doi: 10.1016/s0378-4347(96)00418-5.

DOI:10.1016/s0378-4347(96)00418-5
PMID:9106049
Abstract

The analysis of melarsoprol in whole blood, plasma, urine and cerebrospinal fluid is described. Extraction was made with a mixture of chloroform and acetonitrile followed by back-extraction into phosphoric acid. A reversed-phase liquid chromatography system with ultraviolet detection was used. The relative standard deviation was 1% at concentrations around 10 mumol/l and 3-6% at the lower limit of determination (9 nmol/l in plasma, 93 nmol/l in whole blood, 45 nmol/l in urine and 10 nmol/l in cerebrospinal fluid). Melarsoprol is not a stable compound and samples to be stored for longer periods of time should be kept at -70 degrees C. Plasma samples can be stored at -20 degrees C for up to 2 months. Chromatography showed that melarsoprol contains two components. Using nuclear magnetic resonance spectroscopy the two components were shown to be diastereomers which slowly equilibrate by inversion of the configuration at the As atom.

摘要

本文描述了对全血、血浆、尿液和脑脊液中美拉胂醇的分析方法。用氯仿和乙腈的混合物进行萃取,然后反萃取到磷酸中。采用带紫外检测的反相液相色谱系统。在浓度约为10 μmol/l时,相对标准偏差为1%;在测定下限(血浆中9 nmol/l、全血中93 nmol/l、尿液中45 nmol/l、脑脊液中10 nmol/l)时,相对标准偏差为3 - 6%。美拉胂醇不是一种稳定的化合物,需要长时间保存的样品应保存在 -70℃。血浆样品可在 -20℃保存长达2个月。色谱分析表明美拉胂醇含有两种成分。通过核磁共振光谱法显示这两种成分是非对映异构体,它们通过砷原子构型的翻转而缓慢达到平衡。

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Determination of melarsoprol in biological fluids by high-performance liquid chromatography and characterisation of two stereoisomers by nuclear magnetic resonance spectroscopy.高效液相色谱法测定生物体液中的美拉胂醇并通过核磁共振光谱法表征两种立体异构体
J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):243-51. doi: 10.1016/s0378-4347(96)00418-5.
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