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通过高效液相色谱/质谱法对克拉屈滨及其相关化合物进行表征。

Characterization of cladribine and its related compounds by high-performance liquid chromatography/mass spectrometry.

作者信息

Weber J V, Sampino K, Dunphy R, Burinsky D J, Williams T, Motto M G

机构信息

R.W. Johnson Pharmaceutical Research Institute, Raritan, NJ 08869-0602.

出版信息

J Pharm Sci. 1994 Apr;83(4):525-31. doi: 10.1002/jps.2600830416.

DOI:10.1002/jps.2600830416
PMID:7913965
Abstract

High-performance liquid chromatography/mass spectrometer (HPLC/MS) was used to identify and structurally characterize the modified nucleoside cladribine (2-chloro-2'-deoxy-beta-adenosine) and 13 synthesis-related byproducts in bulk drug. Confirmation of compound identity was accomplished by spectral analysis (1H and 13C NMR spectroscopy, mass spectrometry, and UV absorption spectroscopy) of the related compounds as isolated from crude mixtures of the drug substance and by spiking experiments with authentic standards. The use of on-line mass spectrometric analysis (i.e., LC/MS) to augment UV absorption spectra permitted rapid identification of many of the compounds of interest.

摘要

高效液相色谱/质谱仪(HPLC/MS)用于鉴定和结构表征原料药中修饰核苷克拉屈滨(2-氯-2'-脱氧-β-腺苷)及13种合成相关副产物。通过对从原料药粗混合物中分离出的相关化合物进行光谱分析(1H和13C核磁共振光谱、质谱和紫外吸收光谱)以及用标准品进行加标实验来确认化合物的身份。使用在线质谱分析(即LC/MS)来增强紫外吸收光谱,可快速鉴定许多目标化合物。

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