液相色谱法测定小麦中的麦角生物碱

Liquid chromatographic determination of ergot alkaloids in wheat.

作者信息

Ware G M, Carman A S, Francis O J, Kuan S S

出版信息

J Assoc Off Anal Chem. 1986 Jul-Aug;69(4):697-9.

Abstract

A method is described for the determination of individual ergot alkaloids in wheat. The sample is extracted with ethyl acetate-4% ammonium hydroxide (100 + 10), and the extract is cleaned up by liquid-liquid partition. The ergot alkaloids are resolved by liquid chromatography (LC), using a porous cross-linked polystyrene-divinylbenzene resin column and a mobile phase consisting of acetonitrile-0.05 M dibasic ammonium phosphate (55 + 45) buffered at pH 10.0. The ergot alkaloids ergonovine, ergonovinine, ergotamine, ergotaminine, alpha-ergocryptine, alpha-ergocryptinine, ergocristine, and ergocristinine are separated by LC and detected with a fluorescence detector. Recovery of ergot alkaloids added to wheat at levels of 16-760 ng/g averaged 85.6% with a coefficient of variation of 11.1%.

摘要

描述了一种测定小麦中各麦角生物碱的方法。样品用乙酸乙酯 - 4%氢氧化铵（100 + 10）萃取，提取物通过液 - 液分配进行净化。麦角生物碱通过液相色谱（LC）分离，使用多孔交联聚苯乙烯 - 二乙烯基苯树脂柱和由乙腈 - 0.05M磷酸氢二铵（55 + 45）组成的流动相，在pH 10.0下缓冲。麦角新碱、麦角新宁、麦角胺、麦角胺宁、α - 麦角隐亭、α - 麦角隐亭宁、麦角克碱和麦角克碱宁等麦角生物碱通过LC分离并用荧光检测器检测。添加到小麦中浓度为16 - 760 ng/g的麦角生物碱回收率平均为85.6%，变异系数为11.1%。