用于评估组合文库质量的高效薄层色谱法，以及与液相色谱-紫外-质谱法的比较。

High-performance thin-layer chromatography method for assessment of the quality of combinatorial libraries, and comparison with liquid chromatography-ultraviolet-mass spectrometry.

作者信息

Salo Piia K, Pertovaara Anniina M, Salo Vesa-Markku A, Salomies Hannele E M, Kostiainen Risto K

机构信息

Department of Pharmacy, Division of Pharmaceutical Chemistry, and Viikki Drug Discovery Technology Center, Department of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki, Finland.

出版信息

J Comb Chem. 2003 May-Jun;5(3):223-32. doi: 10.1021/cc020046j.

DOI:10.1021/cc020046j

PMID:12739937

Abstract

A high-performance thin-layer chromatography (HPTLC) method was developed for fast evaluation of the purity of solid-phase synthesis products. The results obtained were in good agreement with results obtained by the LC-MS method (r(2) = 0.8404) or by the LC-UV method (r(2) = 0.8053), confirming the suitability of HPTLC for purity analysis of combinatorial syntheses. The synthesis products can be quantified and identified by measuring UV densitograms or in situ UV spectra or by ESI-MS after isolation of the zone of interest. A new, simple, and fast method for transferring the zone of the analyte from the plate to the ESI-MS equipment is described. The new HPTLC method enables rapid and efficient analysis of approximately 40 samples in parallel. As such, it offers a cheaper and easier way to analyze the purity of synthesis products than the commonly used LC-UV-MS.

摘要

开发了一种高效薄层色谱（HPTLC）方法，用于快速评估固相合成产物的纯度。所得结果与通过液相色谱-质谱法（r(2) = 0.8404）或液相色谱-紫外法（r(2) = 0.8053）获得的结果高度一致，证实了HPTLC适用于组合合成的纯度分析。合成产物可以通过测量紫外光密度图或原位紫外光谱进行定量和鉴定，或者在分离出感兴趣的区域后通过电喷雾电离质谱（ESI-MS）进行分析。描述了一种将分析物区域从平板转移到ESI-MS设备的新的、简单且快速的方法。这种新的HPTLC方法能够并行快速有效地分析约40个样品。因此，与常用的液相色谱-紫外-质谱法相比，它提供了一种更便宜、更简便的分析合成产物纯度的方法。