液质联用分析肉鸡饲料和粪便中伏马菌素 B1、B2、B3 及其水解代谢产物

LC-MS/MS Analysis of Fumonisin B1, B2, B3, and Their Hydrolyzed Metabolites in Broiler Chicken Feed and Excreta.

机构信息

NHC Key Laboratory of Food Safety Risk Assessment, Food Safety Research Unit (2019RU014) of Chinese Academy of Medical Science, China National Center for Food Safety Risk Assessment, Beijing 100021, China.

SIBS-UGENT-SJTU Joint Laboratory of Mycotoxin Research, CAS Key Laboratory of Nutrition, Metabolism and Food Safety, Shanghai Institute of Nutrition and Health, University of Chinese Academy of Sciences, Chinese Academy of Sciences, Shanghai 200031, China.

出版信息

Toxins (Basel). 2022 Feb 9;14(2):131. doi: 10.3390/toxins14020131.

DOI:10.3390/toxins14020131

PMID:35202158

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8875997/

Abstract

An accurate, reliable, and specific method was developed for the quantitative determination of fumonisins B1, B2, B3, and their hydrolyzed metabolites, HFB1, HFB2, and HFB3, in broiler chicken feed and excreta using ultra-performance liquid chromatography combined with tandem mass spectrometry (UPLC-MS/MS). The samples were extracted and diluted for the determination of parent fumonisins. Another portion of the extracted samples was alkaline-hydrolyzed and cleaned using a strong anionic exchange adsorbent (MAX) for the determination of hydrolyzed fumonisins. Chromatographic separation was performed on a CORTECS C18 column (2.1 mm × 100 mm, 1.6 μm) using 0.2% formic acid aqueous solution and methanol with 0.2% formic acid as the mobile phase under gradient elution. The six fumonisins, FB1, FB2, FB3, HFB1, HFB2, and HFB3, were analyzed by tandem mass spectrometry using multiple-reaction monitoring (MRM) mode. The six fumonisins showed good linearity, with relative coefficients of r > 0.99. The limits of quantitation (LOQs) were 160 μg/kg. At the low, medium, and high spiked levels, the recovery of fumonisins in chicken feed and excreta ranged from 82.6 to 115.8%, with a precision (RSD) of 3.9-18.9%. This method was successfully applied to investigate the migration and transformation of fumonisins in broiler chickens.

摘要

建立了一种超高效液相色谱-串联质谱法（UPLC-MS/MS）测定肉鸡饲料和粪便中伏马菌素 B1、B2、B3 及其水解代谢物 HFB1、HFB2、HFB3 的方法。样品经提取和稀释后用于测定母体伏马菌素，提取样品的另一部分经碱性水解，并用强阴离子交换吸附剂（MAX）净化，用于测定水解伏马菌素。色谱分离在 CORTECS C18 柱（2.1mm×100mm，1.6μm）上进行，采用 0.2%甲酸水溶液和甲醇作为流动相，梯度洗脱，在 0.2%甲酸条件下进行洗脱。6 种伏马菌素 FB1、FB2、FB3、HFB1、HFB2、HFB3 采用串联质谱法，以多反应监测（MRM）模式进行分析。6 种伏马菌素均具有良好的线性关系，相关系数 r＞0.99。定量限（LOQ）为 160μg/kg。在低、中、高添加水平下，伏马菌素在鸡饲料和粪便中的回收率为 82.6%～115.8%，精密度（RSD）为 3.9%～18.9%。该方法成功应用于研究伏马菌素在肉鸡中的迁移和转化。