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多功能净化柱和免疫亲和柱联用液相色谱-串联质谱法同时测定黑茶中的四种黄曲霉毒素。

Simultaneous Determination of Four Aflatoxins in Dark Tea by Multifunctional Purification Column and Immunoaffinity Column Coupled to Liquid Chromatography Tandem Mass Spectrometry.

机构信息

State Key Laboratory of Tea Biology and Utilization, School of Tea and Food Science Technology , Anhui Agricultural University , Heifei 230036 , China.

Shanghai Key Laboratory of Bio-Energy Crops , Shanghai University , Shanghai 200444 , China.

出版信息

J Agric Food Chem. 2019 Oct 16;67(41):11481-11488. doi: 10.1021/acs.jafc.9b04933. Epub 2019 Oct 8.

Abstract

Dry tea matrix contains an abundance of caffeine and polyphenols which are different from the food matrix (e.g., protein, lipid, and carbohydrates), and only a few studies have tried aflatoxins determination with tea samples. Here, a specific, accurate, and sensitive method was developed and validated for the simultaneous determination of aflatoxin B1, B2, G1, and G2 in dark teas. Aflatoxins were extracted by acetonitrile/water, press-filtered, and cleaned by multifunctional purification column (MFC) and immunoaffinity column (IAC) in tandem. The cleaned extract was analyzed by liquid chromatography tandem mass spectrometry. The matrix interference was effectively reduced by MFC-IAC cleaning method. Recoveries at the spiking concentrations of 5-60 μg/kg ranged from 77.5 to 93%, with relative standard deviations <11.0%. The correlation coefficients of aflatoxins standard were >0.998. The limits of detection were 0.024-0.21 μg/kg and the limits of quantification were 0.08-0.74 μg/kg. The intra- and interday accuracy ranged from 74 to 87%, and the intra- and interday precisions ranged from 0.4 to 3.1%. After the method validation, the aflatoxins contaminations in 100 collected dark teas were detected, and the results were compared with those of other methods.

摘要

干茶基质中含有丰富的咖啡因和多酚,这些成分与食物基质(如蛋白质、脂质和碳水化合物)不同,只有少数研究尝试过用茶样检测黄曲霉毒素。本研究建立并验证了一种同时检测黑茶中黄曲霉毒素 B1、B2、G1 和 G2 的特异性、准确和灵敏的方法。黄曲霉毒素用乙腈/水提取,加压过滤,经多功能净化柱(MFC)和免疫亲和柱(IAC)串联净化,用液相色谱串联质谱法分析。MFC-IAC 净化方法有效降低了基质干扰。在 5-60μg/kg 的添加浓度下,回收率在 77.5-93%之间,相对标准偏差<11.0%。黄曲霉毒素标准的相关系数>0.998。检测限为 0.024-0.21μg/kg,定量限为 0.08-0.74μg/kg。日内和日间准确度范围为 74-87%,日内和日间精密度范围为 0.4-3.1%。方法验证后,检测了 100 份采集的黑茶中的黄曲霉毒素污染情况,并与其他方法的结果进行了比较。

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