中文摘要：近年来，用生物标记评估真菌毒素暴露的策略得到了越来越多的认可。本研究研制了一种用96孔微洗脱固相萃取改进并验证的UPLC-MS/MS法，以13C-ZEN为内标进行准确定量，用来高通量灵敏测定人尿中的玉米赤霉烯酮（ZEN）及其五种代谢物，α-玉米赤霉烯醇(α-ZEL)、β-玉米赤霉烯醇(β-ZEL)、α-玉米赤霉醇(α-ZAL)、β-玉米赤霉醇(β-ZAL)以及玉米赤霉酮(ZAN)。研究表明，估算的平均每日可能摄入量(PDI)远低于每日容许摄入量(TDI)；青少年的暴露水平高于儿童、成人和老年人。
外文摘要：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 μElution solid-phase extraction was developed and validated for the sensitive and high-throughput determination of zearalenone (ZEN) and its five metabolites α-zearalenol (α-ZEL), β-zearalenol (β-ZEL), α-zearalanol (α-ZAL), β-zearalanol (β-ZAL), and zearalanone (ZAN) in human urine samples, using 13C-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, α-ZEL, and β-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.
外文关键词：Biomonitoring；Zearalenone；Metabolites；Urine；96-well mu Elution SPE；UPLC-MS/MS
作者：Li, CL；Deng, CL；Zhou, S；Zhao, YF；Wang, D；Wang, XD；Gong, YY；Wu, YN
作者单位：China Natl Ctr Food Safety Risk Assessment
期刊名称：ANALYTICAL AND BIOANALYTICAL CHEMISTRY
期刊影响因子：3.125
出版年份：2018
出版刊次：21
点击下载：用UPLC-MS/MS法高通量灵敏测定尿液玉米赤霉烯醇及其代谢物以及该方法在人体暴露研究中的应用