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采用 LC-MS/MS 分析苦马豆素的替代样品制备程序比较。

A comparison of alternative sample preparation procedures for the analysis of swainsonine using LC-MS/MS.

机构信息

USDA, ARS, Poisonous Plant Research Laboratory, 1150 E. 1400 N., Logan, Utah, USA.

出版信息

Phytochem Anal. 2011 Mar-Apr;22(2):124-7. doi: 10.1002/pca.1257. Epub 2010 Aug 26.

Abstract

INTRODUCTION

Swainsonine, a polyhydroxy indolizidine alkaloid and known glycosidase inhibitor, is found in a number of different plants that cause a lysosomal storage disease known as locoism in the western USA. Most recently swainsonine has been analysed by LC-MS/MS after sample extraction and preparation from ion-exchange resins.

OBJECTIVE

To compare previously published sample preparation procedures with several new alternative procedures to provide methods using either commercially available solid-phase extraction equipment or procedures which significantly reduce sample preparation time.

METHODOLOGY

A previously reported and validated sample preparation method using ion-exchange resin was compared with methods using a commercially available solid-phase extraction cartridge, a solvent partitioning procedure or a single solvent extraction procedure using one of two solvents. Twenty different plant samples of varying swainsonine concentrations were prepared in triplicate and analysed by LC-MS/MS. The measured concentration of swainsonine was then statistically compared between methods.

RESULTS

There were no statistically significant differences found between four of the five different sample preparation methods tested.

CONCLUSION

A commercially available SPE cartridge can be used to replace the previously used ion-exchange resin for swainsonine analysis. For very rapid analyses the SPE procedure can be eliminated and a simple, single solvent extraction step used for sample preparation.

摘要

简介

苦马豆素是一种多羟基吲哚里西啶生物碱和已知的糖苷酶抑制剂,存在于许多不同的植物中,这些植物在美国西部引起一种溶酶体贮积病,称为 loco 病。最近,苦马豆素已通过 LC-MS/MS 进行了分析,样品经过离子交换树脂提取和制备。

目的

将以前发表的样品制备程序与几种新的替代程序进行比较,提供使用商业上可获得的固相萃取设备或显著减少样品制备时间的程序的方法。

方法

比较了一种以前报道并经过验证的使用离子交换树脂的样品制备方法与使用商业上可获得的固相萃取小柱、溶剂分配程序或使用两种溶剂之一的单一溶剂萃取程序的方法。用三种方法制备了 20 种不同苦马豆素浓度的植物样品,并通过 LC-MS/MS 进行分析。然后对方法之间的苦马豆素测量浓度进行了统计学比较。

结果

在测试的五种不同样品制备方法中,有四种方法之间没有统计学上的显著差异。

结论

可以使用商业上可获得的固相萃取小柱代替以前使用的离子交换树脂进行苦马豆素分析。对于非常快速的分析,可以省略 SPE 程序,并使用简单的单一溶剂萃取步骤进行样品制备。

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