PMID- 29951770 OWN - NLM STAT- MEDLINE DCOM- 20180814 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 410 IP - 21 DP - 2018 Aug TI - High-throughput and sensitive determination of urinary zearalenone and metabolites by UPLC-MS/MS and its application to a human exposure study. PG - 5301-5312 LID - 10.1007/s00216-018-1186-4 [doi] AB - Biomarker-based strategies to assess human exposure to mycotoxins have gained increased acceptance in recent years. In this study, an improved method based on UPLC-MS/MS following 96-well muElution solid-phase extraction was developed and validated for the sensitive and high-throughput determination of zearalenone (ZEN) and its five metabolites alpha-zearalenol (alpha-ZEL), beta-zearalenol (beta-ZEL), alpha-zearalanol (alpha-ZAL), beta-zearalanol (beta-ZAL), and zearalanone (ZAN) in human urine samples, using (13)C-ZEN as an internal standard for accurate quantification. Two plates of samples (n = 192) could be processed within 2 h, and baseline separation of all the analytes was achieved in a total runtime of 6 min. The proposed method allowed ZEN and its metabolites to be sensitively determined in a high-throughput way for the first time, and with significantly improved efficiency and accuracy with respect to existing methods. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.02 to 0.06 ng mL(-1) and from 0.05 to 0.2 ng mL(-1), respectively. The recoveries for the spiked samples were from 87.9 to 100%, with relative standard deviations (RSDs) of less than 7%. 301 urine samples collected from healthy volunteers aged 0-84 years in China were analyzed with and without enzyme hydrolysis to determine total and free ZEN biomarkers, respectively. ZEN, ZAN, alpha-ZEL, and beta-ZEL were detected in 71.4% of the samples at levels of 0.02-3.7 ng mL(-1) after enzyme hydrolysis. The estimated mean probable daily intake (PDI) was much lower than the tolerable daily intake (TDI). Adolescents had higher exposure than children, adults, and the elderly. Graphical abstract ᅟ. FAU - Li, Chenglong AU - Li C AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. FAU - Deng, Chunli AU - Deng C AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. FAU - Zhou, Shuang AU - Zhou S AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. szhoupku@gmail.com. FAU - Zhao, Yunfeng AU - Zhao Y AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. FAU - Wang, Dan AU - Wang D AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. FAU - Wang, Xiaodan AU - Wang X AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. FAU - Gong, Yun Yun AU - Gong YY AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. AD - School of Food Science and Nutrition, University of Leeds, Woodhouse Ln, Leeds, LS2 9JT, UK. FAU - Wu, Yongning AU - Wu Y AD - China National Center for Food Safety Risk Assessment, Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing, 100021, China. LA - eng GR - 31501400/National Natural Science Foundation of China/ PT - Journal Article PT - Validation Study DEP - 20180627 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Estrogens, Non-Steroidal) RN - 5W827M159J (Zearalenone) SB - IM MH - Adolescent MH - Adult MH - Aged MH - Aged, 80 and over MH - Child MH - Child, Preschool MH - Chromatography, High Pressure Liquid/*methods MH - Estrogens, Non-Steroidal/metabolism/*urine MH - Female MH - High-Throughput Screening Assays/methods MH - Humans MH - Infant MH - Limit of Detection MH - Male MH - Middle Aged MH - Solid Phase Extraction/methods MH - Tandem Mass Spectrometry/*methods MH - Young Adult MH - Zearalenone/metabolism/*urine OTO - NOTNLM OT - 96-well muElution SPE OT - Biomonitoring OT - Metabolites OT - UPLC-MS/MS OT - Urine OT - Zearalenone EDAT- 2018/06/29 06:00 MHDA- 2018/08/15 06:00 CRDT- 2018/06/29 06:00 PHST- 2017/12/27 00:00 [received] PHST- 2018/06/05 00:00 [accepted] PHST- 2018/05/28 00:00 [revised] PHST- 2018/06/29 06:00 [pubmed] PHST- 2018/08/15 06:00 [medline] PHST- 2018/06/29 06:00 [entrez] AID - 10.1007/s00216-018-1186-4 [pii] AID - 10.1007/s00216-018-1186-4 [doi] PST - ppublish SO - Anal Bioanal Chem. 2018 Aug;410(21):5301-5312. doi: 10.1007/s00216-018-1186-4. Epub 2018 Jun 27.