超薄层色谱 - 质谱法和血管紧张素转化酶抑制剂单肽的薄层色谱 - 质谱法。

Ultra-thin-layer chromatography mass spectrometry and thin-layer chromatography mass spectrometry of single peptides of angiotensin-converting enzyme inhibitors.

机构信息

National Institute of Chemistry, Laboratory for Food Chemistry, Ljubljana, Slovenia.

出版信息

J Chromatogr A. 2011 May 20;1218(20):3089-94. doi: 10.1016/j.chroma.2011.03.039. Epub 2011 Apr 13.

DOI:10.1016/j.chroma.2011.03.039

Abstract

The separation of structurally related angiotensin-converting enzyme (ACE) inhibitors lisinopril, cilazapril, ramipril and quinapril and their corresponding active diacid forms (prilates) by conventional TLC silica gel 60 plates was contrasted with that afforded by monolithic ultra-thin-layer chromatographic (UTLC) plates. For the use of UTLC plates technical modifications of the commercially available equipments for the sample application, development and detection were made. Plates were developed in modified horizontal developing chamber using ethyl acetate-acetone-acetic acid-water (4:1:0.25:0.5, v/v). Detection of the separated compounds was performed densitometrically in absorption/reflectance mode at 220 nm and after exposure to iodine also by image analysis. The obtained results showed that monolithic layer is more efficient for the separation of structurally similar polar compounds, such as prilates than conventional silica layers. Identification of the compounds was confirmed by ESI-MS after their on-line extraction from the UTLC and TLC plates by means of Camag TLC-MS interface.

摘要

将结构相关的血管紧张素转换酶（ACE）抑制剂（如赖诺普利、西拉普利、雷米普利和喹那普利）及其相应的活性二羧酸形式（普利拉）与传统的 TLC 硅胶 60 板进行分离，并与整体式超薄层色谱（UTLC）板提供的分离方法进行对比。为了使用 UTLC 板，对商业上可用于样品应用、开发和检测的设备进行了技术修改。在改良的水平展开室中，使用乙酸乙酯-丙酮-冰醋酸-水（4:1:0.25:0.5，v/v）展开板。在 220nm 处通过吸光度/反射率模式进行分离化合物的检测，并且在暴露于碘后也可以通过图像分析进行检测。结果表明，与传统的硅胶层相比，整体层对于分离结构相似的极性化合物（如普利拉）更为有效。通过 Camag TLC-MS 接口，从 UTLC 和 TLC 板上在线提取化合物后，通过 ESI-MS 对化合物进行鉴定。