采用固相净化和窄径液相色谱 - 荧光检测器 - 质谱联用技术分析咖啡中的赭曲霉毒素A。

Analysis of ochratoxin a in coffee by solid-phase cleanup and narrow-bore liquid chromatography-fluorescence detector-mass spectrometry.

作者信息

Ventura Meritxell, Vallejos Carlos, Anaya Iván Atilio, Broto-Puig Francesc, Agut Montserrat, Comellas Lluís

机构信息

Analytical Chemistry Department, Institut Químic de Sarrià, Ramon Llull University, Via Augusta 390, 08017 Barcelona, Spain.

出版信息

J Agric Food Chem. 2003 Dec 17;51(26):7564-7. doi: 10.1021/jf034856+.

DOI:10.1021/jf034856+

PMID:14664508

Abstract

A method for the analysis of ochratoxin A (OTA) in green and roasted coffee has been developed. OTA was extracted from coffee with 1% NaHCO(3), and the extract was filtered and purified by solid-phase cleanup using a polymeric column that exhibits reversed-phase and anion-exchange functionalities. OTA was analyzed on a narrow-bore reversed-phase C(18) HPLC column with acetonitrile/water (0.1% formic acid) (40:60) as mobile phase and quantified with a fluorescence detector. The presence of OTA in coffee was confirmed by single-quadruple mass spectrometry using an electrospray ionization source. The method has been validated, obtaining a recovery of 82.5% and a detection limit of 0.1 ng/g. It has been applied to 20 coffee samples from various countries and different manufacturers with no detection of OTA.

摘要

已开发出一种分析生咖啡和烘焙咖啡中赭曲霉毒素A（OTA）的方法。用1%碳酸氢钠从咖啡中提取OTA，提取物经过滤后，使用具有反相和阴离子交换功能的聚合物柱进行固相净化。在窄孔反相C18高效液相色谱柱上分析OTA，以乙腈/水（0.1%甲酸）（40:60）作为流动相，并用荧光检测器进行定量。使用电喷雾电离源的单四极杆质谱法确认了咖啡中OTA的存在。该方法已经过验证，回收率为82.5%，检测限为0.1 ng/g。该方法已应用于来自不同国家和不同制造商的20个咖啡样品，未检测到OTA。