Development and validation of an LC-MS/MS method for the toxicokinetic study of deoxynivalenol and its acetylated derivatives in chicken and pig plasma
Development and validation of an LC-MS/MS method for the toxicokinetic study of deoxynivalenol and its acetylated derivatives in chicken and pig plasma
复制标题
DOI：
10.1016/j.jchromb.2014.09.012
复制
发表时间：
2014-11-15
影响因子：
3
通讯作者：
Croubels, S.
中科院分区：
文献类型：
--
作者：
Broekaert, N.;Devreese, M.;Croubels, S.
本研究建立了测定肉鸡和猪体内3-乙酰-脱氧雪腐镰刀菌烯醇、15-乙酰-脱氧雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇及其体内主要代谢物脱氧-脱氧雪腐镰刀菌烯醇的LC-MS/MS方法。考虑到这些物种主要以谷物为主的饮食，它们对这些毒素的暴露程度很高。通过部分析因设计对几种样品清理策略进行了测试和进一步优化。开发了一种简单直接的样品制备方法，包括用乙腈脱蛋白的步骤，然后蒸发上清液并在水中重新组成。根据欧洲指南对该方法进行了单一实验室验证，发现该方法适用于预期目的，线性响应高达200 ng ml(-1)，定量限为0.1-2 ng ml(-1)。作为概念的验证，来自肉鸡的生物样本被分析了，这些肉鸡接受了脱氧雪腐镰刀菌烯醇、3-或15-乙酰脱氧雪腐镰刀菌烯醇。初步结果表明，3-乙酰基-脱氧雪腐镰刀菌烯醇几乎完全水解为脱氧雪腐镰刀菌烯醇；15-乙酰基-脱氧雪腐镰刀菌烯醇几乎完全水解为脱氧雪腐镰刀菌烯醇。在所有血浆样本中均未检测到脱氧雪腐镰刀菌烯醇。该方法将用于研究脱氧雪腐镰刀菌烯醇、3-乙酰-脱氧雪腐镰刀菌烯醇和15-乙酰基-脱氧雪腐镰刀菌烯醇在肉鸡和猪体内的完整毒代动力学特性。(C)2014爱思唯尔B.V.保留所有权利。
This study aims to develop an LC-MS/MS method allowing the determination of 3-acetyl-deoxynivalenol, 15-acetyl-deoxynivalenol, deoxynivalenol and its main in vivo metabolite, deepoxy-deoxynivalenol, in broiler chickens and pigs. These species have a high exposure to these toxins, given their mainly cereal based diet. Several sample cleanup strategies were tested and further optimized by means of fractional factorial designs. A simple and straightforward sample preparation method was developed consisting out of a deproteinisation step with acetonitrile, followed by evaporation of the supernatant and reconstitution in water. The method was single laboratory validated according to European guidelines and found to be applicable for the intended purpose, with a linear response up to 200 ng ml(-1) and limits of quantification of 0.1-2 ng ml(-1). As a proof of concept, biological samples from a broiler chicken that received either deoxynivalenol, 3- or 15-acetyl-deoxynivalenol were analyzed. Preliminary results indicate nearly complete hydrolysis of 3-acetyl-deoxynivalenol to deoxynivalenol; and to a lesser extent of 15-acetyl-deoxynivalenol to deoxynivalenol. No deepoxy-deoxynivalenol was detected in any of the plasma samples. The method will be applied to study full toxicokinetic properties of deoxynivalenol, 3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol in broiler chickens and pigs. (C) 2014 Elsevier B.V. All rights reserved.