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利用 PLE 和 HPLC-MS/MS 对人及实验动物生物体液和组织中的多种真菌毒素进行高通量同步检测的方法。

A high-throughput method for the simultaneous determination of multiple mycotoxins in human and laboratory animal biological fluids and tissues by PLE and HPLC-MS/MS.

机构信息

Department of Pharmacy, Wuhan University, Wuhan 430072, People's Republic of China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Dec 30;942-943:113-25. doi: 10.1016/j.jchromb.2013.10.017. Epub 2013 Oct 21.

DOI:10.1016/j.jchromb.2013.10.017
PMID:24239936
Abstract

A high-throughput method for the determination of 28 mycotoxins involving pressurised liquid extraction (PLE) coupled with liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been optimised and validated for determination in various biological fluids and tissues of human and laboratory animals. High-throughput analysis was achieved using PLE pre-treatment and without the need for any cleanup. The extraction solvent was acetonitrile/water/acetic acid (80/19/1, v/v/v). The static extraction time was 5min. The extraction pressure and temperature were 1500psi and 140°C, respectively. The flush volume was 60%. The limits of detection, which were defined as CCα, varied from 0.01μg/kg (μg/L) to 0.69μg/kg (μg/L). The recoveries of spiked samples from 0.20μg/kg (μg/L) to 2μg/kg (μg/L) ranged from 71% to 100.5% with relative standard deviations of less than 17.5%, except FB1 and FB2 recoveries, which were lower than 60%. The method was successfully applied in real samples, and the data indicate that this technique is a useful analytical method for the determination of mycotoxins from humans and animals. To the best of our knowledge, this method is the first for the large-scale testing of multi-class mycotoxins in all types of biological fluids and tissues that uses PLE and HPLC-MS/MS.

摘要

一种涉及加压液体萃取(PLE)与液相色谱-串联质谱(HPLC-MS/MS)联用的高通量方法,已被优化并验证可用于检测人类和实验动物的各种生物体液和组织中的 28 种霉菌毒素。高通量分析采用 PLE 预处理,无需任何净化。萃取溶剂为乙腈/水/乙酸(80/19/1,v/v/v)。静态萃取时间为 5min。萃取压力和温度分别为 1500psi 和 140°C。冲洗体积为 60%。检测限(CCα)定义为 0.01μg/kg(μg/L)至 0.69μg/kg(μg/L)。从 0.20μg/kg(μg/L)至 2μg/kg(μg/L)添加的样品的回收率在 71%至 100.5%之间,相对标准偏差小于 17.5%,除 FB1 和 FB2 的回收率低于 60%。该方法已成功应用于实际样品,数据表明该技术是一种用于检测人类和动物中霉菌毒素的有用分析方法。据我们所知,这是第一种使用 PLE 和 HPLC-MS/MS 对所有类型的生物体液和组织中的多类霉菌毒素进行大规模检测的方法。

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