超高效液相色谱/串联质谱联用超声提取法测定加工谷物产品中的赭曲霉毒素A

Ultrasonic extraction with ultra-performance liquid chromatography/tandem mass spectrometry for the determination of ochratoxin A in processed cereal products.

作者信息

Nguyen Kieu Thi Ngoc, Ryu Dojin

机构信息

University of Idaho, School of Food Sciences, 875 Perimeter Dr, MS 2312, Moscow, ID 83844-2312, USA.

出版信息

J AOAC Int. 2014 Sep-Oct;97(5):1384-6. doi: 10.5740/jaoacint.13-425.

DOI:10.5740/jaoacint.13-425

PMID:25902987

Abstract

A rapid, simple, and reliable method using ultra-performance LC/MS/MS (UPLC/MS/MS) was developed for determination of ochratoxin A (OTA) in processed cereal products. OTA was ultrasonically extracted from the sample with acetonitrile-water (80 + 20, v/v), and the extract was then injected into the UPLC/MS/MS system after filtration. The calibration curves had good linearity with coefficients of determination greater than 0.999. Recoveries of OTA were in the range of 90-104%. LOD and LOQ of OTA in samples were 0.6 and 2.0 ng/g, respectively, and no significant matrix effect was found. This method was applied to determine OTA in 25 oat-based cereal samples. OTA was detected in five samples (20%) in the range of 2.4 to 7.3 ng/g.

摘要

建立了一种快速、简单且可靠的超高效液相色谱-串联质谱法（UPLC/MS/MS），用于测定加工谷物制品中的赭曲霉毒素A（OTA）。用乙腈-水（80 + 20，v/v）从样品中超声提取OTA，提取液过滤后注入UPLC/MS/MS系统。校准曲线具有良好的线性，决定系数大于0.999。OTA的回收率在90%-104%之间。样品中OTA的检测限和定量限分别为0.6 ng/g和2.0 ng/g，且未发现明显的基质效应。该方法用于测定25份燕麦基谷物样品中的OTA。在5份样品（20%）中检测到OTA，含量在2.4至7.3 ng/g之间。