Quantitative determination of mycotoxins in urine by LC-MS/MS
Quantitative determination of mycotoxins in urine by LC-MS/MS
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DOI：
10.1080/19440049.2010.505201
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发表时间：
2010-01-01
影响因子：
2.9
通讯作者：
Jahng, K. -Y.
中科院分区：
文献类型：
--
作者：
Ahn, J.;Kim, D.;Jahng, K. -Y.
天然存在的霉菌毒素会对健康产生多种不良影响。尿液霉菌毒素水平的测量是评估个体接触情况的有用方法，但开发用于检测尿液样本中霉菌毒素及其代谢物的灵敏且准确的分析方法具有挑战性。尿液中霉菌毒素的浓度较低，为 pg ml-1，其代谢物的色谱鉴定可能会被其他内源性代谢物所掩盖。我们开发了一种分析方法，重点是选择两种适当的多反应监测转换，以明确鉴定和定量试点研究中一小群志愿者尿液样本中的致癌黄曲霉毒素 M1 (AFM1)、赭曲霉毒素 A (OTA) 和伏马菌素 B1、B2 (FB1、FB2)。选择性浓缩 AFM1、OTA、FB1 和 FB2，使用免疫亲和柱 (IAC) 去除干扰物质，并使用液相色谱-串联质谱 (LC-MS/MS) 结合稳定同位素标准稀释测定 (SIDA) 测量霉菌毒素。该方法足够灵敏，可以测量尿液中 pg ml-1 水平的霉菌毒素及其代谢物。 LC-MS/MS 和 SIDA 的结合对于区分伪 OT 干扰和真正 OT 至关重要。 12 份尿液样本中 OTA 含量范围为 0.013 至 0.093 ng ml-1（平均值 = 0.031 ng ml-1）。在一份样品中检测到 0.002 ng ml-1 水平的 AFM1，而在所有 12 个样品中均检测不到 FB1 和 FB2。尽管存在 OTA，但本试点研究中的样本均未检测到 OT 水平，这可能表明需要对韩国人群中 OTA 暴露进行进一步的流行病学调查。
Naturally occurring mycotoxins are responsible for a wide array of adverse health effects. The measurement of urinary mycotoxin levels is a useful means of assessing an individual's exposure, but the development of sensitive and accurate analytical methods for detecting mycotoxins and their metabolites in urine samples is challenging. Urinary mycotoxins are present in low pg ml-1 concentrations, and the chromatographic identification of their metabolites can be obscured by other endogenous metabolites. We developed an analytical method focused on the selection of two appropriate multiple-reaction monitoring transition for unambiguous identification and quantification of carcinogenic aflatoxin M1 (AFM1), ochratoxin A (OTA) and fumonisin B1, B2 (FB1, FB2) in urine samples from a small volunteer group in a pilot study. AFM1, OTA, FB1 and FB2 were concentrated selectively, interfering substances were removed using an immunoaffinity column (IAC), and mycotoxins were measured using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in combination with a stable-isotope standard-dilution assay (SIDA). The method was sensitive enough to measure mycotoxins and their metabolites at pg ml-1 levels in urine. The combination of LC-MS/MS and SIDA was critical to distinguishing pseudo-OT interference from genuine OT. Twelve urine samples contained OTA ranging from 0.013 to 0.093 ng ml-1 (mean = 0.031 ng ml-1). AFM1 were detected in one sample at a 0.002 ng ml-1 level, while FB1 and FB2 were undetectable in all 12 samples. None of the samples in this pilot study contained a detectable level of OT, despite the presence of OTA, and this may suggest the need for further epidemiological investigation of OTA exposure in the Korean population.