SIBS-UGENT-SJTU Joint Laboratory of Mycotoxin Research, Key Laboratory of Food Safety Research, Shanghai Institutes for Biological Sciences, University of Chinese Academy of Sciences, Chinese Academy of Sciences, Shanghai 200000, China.
Academy of State Administration of Grain P.R.C, No. 11 Baiwanzhuang Avenue, Xicheng District, Beijing 100037, China.
Toxins (Basel). 2018 Mar 20;10(3):129. doi: 10.3390/toxins10030129.
The determination of zearalenone (ZEN) and its derivatives as biomarkers in animal tissues or organs plays an important role in mycotoxin monitoring and can promote effective exposure assessment. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantification of nine ZEN-like mycotoxins, including three glucuronides in different pig tissues (heart, liver, spleen and muscle) was developed and validated in this study. Tissue samples were extracted using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and clean-up procedure, and analyzed by LC-MS/MS in multiple reaction monitoring (MRM) mode. Dynamic linear ranges for each target analyte were determined with ² between 0.916 and 0.999. The LODs of the six ZENs were achieved in the range of 0.5-1 ng/g and the LOQs varied from 1 ng/g to 2 ng/g. The satisfying intra-day and inter-day reproducibility (both RSD and RSD < 20%) indicated a good stability of this method. The recoveries of the nine target analytes were in the range of 70-110%. The validation results showed that this LC-MS/MS method coupled with QuEChERS sample pretreatment is effective and suitable for the simultaneous quantitation of ZEN metabolites in pigs. It has been applied to analysis of the pig tissues in this research and can be also adapted for samples in the mycotoxin research field.
本研究建立并验证了一种同时测定猪心、肝、脾和肌肉等不同组织中 9 种 ZEN 类似物真菌毒素(包括 3 种不同结合形式的葡糖苷酸)的液相色谱-串联质谱(LC-MS/MS)检测方法。采用快速、简单、廉价、有效、耐用和安全(QuEChERS)提取和净化方法提取组织样品,然后在多反应监测(MRM)模式下进行 LC-MS/MS 分析。每个目标分析物的动态线性范围在 0.916 至 0.999 之间。6 种 ZEN 的检出限(LOD)在 0.5-1ng/g 范围内,定量限(LOQ)在 1-2ng/g 之间。日内和日间精密度(RSD 和 RSD < 20%)良好,表明该方法稳定性良好。9 种目标分析物的回收率在 70-110%之间。验证结果表明,该 LC-MS/MS 方法结合 QuEChERS 样品预处理有效且适用于同时定量测定猪体内 ZEN 代谢物。该方法已应用于本研究中猪组织的分析,也可适用于真菌毒素研究领域的样品。