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A direct assessment of mycotoxin biomarkers in human urine samples by liquid chromatography tandem mass spectrometry

文献类型： 外文期刊

作者： Ediage, Emmanuel Njumbe 1 ; Di Mavungu, Jose Diana 1 ; Song, Suquan 1 ; Wu, Aibo 2 ; Van Peteghem, Carlos 1 ; De Sa 1 ;

作者机构： 1.Univ Ghent, Dept Bioanal, Lab Food Anal, B-9000 Ghent, Belgium

2.Shanghai Acad Agr Sci, Inst Agrifood Stand & Testing Technol, Lab Mycotoxin Res, Shanghai 201403, Peoples R China

关键词： Mycotoxin;Biomarkers;Urine;Glucuronide;Experimental design;Stability study

期刊名称：ANALYTICA CHIMICA ACTA （ 影响因子：6.558； 五年影响因子：6.228 ）

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收录情况： SCI

摘要： Detection of mycotoxin biomarkers in urine of humans and animals provides a direct approach for assessing exposure to these mycotoxins as opposed to the indirect approach of food analysis, which in most cases is affected by the heterogeneity of the toxin in the food samples. Seven (7) mycotoxins and their metabolites (total 18 analytes) were selected and an LC-MS/MS method for their determination in human urine was developed and validated. The method consisted of direct analysis of two mycotoxin conjugates, deoxynivalenol-glucuronide and zearalenone-glucuronide without beta glucuronidase digestion of the urine samples. Since high method sensitivity is of utmost importance in such study, critical factors which could improve the analyte recovery and method sensitivity were investigated by a D-optimal experimental design. Urine samples (10mL) were first extracted with 15mL ethyl acetate/formic acid (99/1, v/v) followed by SAX SPE clean-up of the acidified aqueous fraction. Both extracts were combined and analyzed using an LC-MS/MS system operated in the positive ionization mode. A total run time of 28 min was adopted with all the 18 analytes eluting within 15 min. The method was validated by taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 401/2006/EC Forty samples obtained from volunteers within the laboratory research group were analyzed as part of a pilot study. All results were expressed per mg creatinine. A total of 9 samples were found contaminated with one or more of the following analytes: DON, OTA, OTa, 4-OH OTA, ZEN, CFT and β-ZOL One-eighth (5/40) of the samples were contaminated with DON in the range of 3.7-67 ng mg~(-1) creatinine. Samples with detectable levels of DON did not show any co-occurrence of DON-3Glu. One sample was found to be contaminated with 4-OH OTA (

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