建立并验证一种 LC-MS/MS 方法，用于同时检测多种饲料和食品中的桔青霉素和赭曲霉毒素 A。

Development and validation of an LC-MS/MS method for the simultaneous determination of citrinin and ochratoxin a in a variety of feed and foodstuffs.

机构信息

Ghent University, Department of Bioanalysis, Centre of Excellence in Mycotoxicology and Public Health, Ottergemsesteenweg 460, 9000 Ghent, Belgium; Ghent University, Department of Pharmacology, Toxicology and Biochemistry, Salisburylaan 133, 9820 Merelbeke, Belgium.

Ghent University, Department of Bioanalysis, Centre of Excellence in Mycotoxicology and Public Health, Ottergemsesteenweg 460, 9000 Ghent, Belgium.

出版信息

J Chromatogr A. 2018 Dec 14;1580:100-109. doi: 10.1016/j.chroma.2018.10.039. Epub 2018 Oct 22.

DOI:10.1016/j.chroma.2018.10.039

PMID:30384965

Abstract

An ultra-performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS) method for the simultaneous analysis of citrinin (CIT) and ochratoxin A (OTA) in feed (chicken and pig) and food (cereal-based products, fruit, vegetable juices, nuts, seeds, herbs, spices, vegetarian and soy products, alcoholic beverages, baby food products and food supplements) was developed. The mycotoxins were extracted from these matrices using a QuEChERS-based extraction method without any further clean-up step. The samples were 5-fold concentrated. Final extracts were analyzed using a UPLC-MS/MS system and chromatographic separation was achieved by applying a gradient elution for a total run time of 10 min. Mycotoxins were quantified using an internal calibration via analyte/C-labeled internal standard ratio. The developed method was validated according to the criteria described in Commission Regulation No. 401/2006/EC and Commission Decision No. 2002/657/EC. Specificity, linearity, apparent recovery, limit of detection and quantification, intraday and interday precision, measurement uncertainty, matrix effect, and extraction efficiency were the parameters studied. Finally, 90 Belgian chicken and pig feed samples were analyzed, revealing the simultaneous presence of CIT (<LOQ - 3.90 μg/kg) and OTA (<LOQ - 5.60 μg/kg) in more than 50% of these products.

摘要

建立了一种同时检测饲料（鸡和猪）和食品（谷物制品、水果、蔬菜汁、坚果、种子、草药、香料、素食和豆制品、酒精饮料、婴儿食品和食品补充剂）中桔青霉素（CIT）和赭曲霉毒素 A（OTA）的超高效液相色谱-电喷雾串联质谱法（UPLC-ESI-MS/MS）。采用基于 QuEChERS 的提取方法，无需进一步净化步骤，从这些基质中提取真菌毒素。样品经过 5 倍浓缩。最终提取物采用 UPLC-MS/MS 系统进行分析，采用梯度洗脱，总运行时间为 10 min 实现色谱分离。通过分析物/C 标记内标比率进行内部校准来定量真菌毒素。根据委员会法规 No. 401/2006/EC 和委员会决定 No. 2002/657/EC 的标准对开发的方法进行了验证。研究了专属性、线性、表观回收率、检测限和定量限、日内和日间精密度、测量不确定度、基质效应和提取效率。最后，分析了 90 份比利时鸡和猪饲料样品，发现这些产品中超过 50%同时存在 CIT（<LOQ - 3.90 μg/kg）和 OTA（<LOQ - 5.60 μg/kg）。