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建立并验证超高效液相色谱-串联质谱法同时测定血浆和尿液中两种交链孢霉毒素及其代谢物的定量分析方法。

Development and validation of a simultaneous quantitative analytical method for two Alternaria toxins and their metabolites in plasma and urine using ultra-high-performance liquid chromatography-tandem mass spectrometry.

机构信息

Department of Inspection and Quarantine, School of Public Health, Anhui Medical University, Hefei, China.

Physical and Chemical Laboratory, Anhui Provincial Center for Disease Control and Prevention, Hefei, China.

出版信息

J Sep Sci. 2024 Jun;47(12):e2400223. doi: 10.1002/jssc.202400223.

Abstract

Much more attention has been paid to the contamination of Alternaria toxins because of food contamination and the threat to human health. In this study, an ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for the simultaneous detection of the prototypical alternariol, alternariol monomethylether, and the metabolites 4-oxhydryl alternariol, and alternariol monomethylether 3-sulfate ammonium salt of Alternaria toxins. The positive samples were used as matrix samples to optimize the different experimental conditions. 0.01% formic acid solution and acetonitrile were used as the mobile phase, and analytes were scanned in negative electron spray ionization under multiple reaction monitoring, and quantitative determination by isotope internal standard method. Application of this method to samples of human plasma and urine showed the detection of the above analytes. The results showed that the recoveries were from 80.40% to 116.4%, intra-day accuracy was between 0.6% and 8.0%, and inter-day accuracy was between 1.1% and 12.1%. The limit of detection of the four analytes ranged from 0.02 to 0.6 µg/L in urine, and 0.02 to 0.5 µg/L in plasma, respectively. Thus, the developed method was rapid and accurate for the simultaneous detection of analytes and provided a theoretical basis for the risk assessment of Alternaria toxins for human exposure.

摘要

由于食品污染和对人类健康的威胁,人们更加关注交链孢霉毒素的污染。在这项研究中,建立了一种超高效液相色谱-串联质谱法,用于同时检测典型的交链孢酚、交链孢酚单甲醚和代谢产物 4-羟化交链孢酚、交链孢酚单甲醚 3-硫酸盐铵盐的交链孢霉毒素。阳性样品被用作基质样品,以优化不同的实验条件。以 0.01%甲酸溶液和乙腈为流动相,在负离子电喷雾电离下以多反应监测模式进行扫描,并采用同位素内标法进行定量测定。将该方法应用于人血浆和尿液样品中,检测到上述分析物。结果表明,回收率在 80.40%至 116.4%之间,日内准确度在 0.6%至 8.0%之间,日间准确度在 1.1%至 12.1%之间。四种分析物在尿液中的检测限为 0.02 至 0.6µg/L,在血浆中的检测限为 0.02 至 0.5µg/L。因此,该方法快速、准确,可用于同时检测分析物,为评估人类暴露于交链孢霉毒素的风险提供了理论依据。

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