炒麦芽中黄曲霉毒素污染状况及其向茶汤中的迁移研究

Study on aflatoxins contamination in processed Hordei Fructus Germinatus and their transfer into tea

目的采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定炒麦芽中的黄曲霉毒素B1、B2、G1、G2,进行状况调查并考察其从炒麦芽向茶汤中的迁移率。方法以13C-稳定同位素标记的黄曲霉毒素为内标,采用免疫亲和柱净化样品,HPLC-MS/MS法测定炒麦芽中黄曲霉毒素B1、B2、G1、G2的含量,并进行方法验证;用该方法对72个批次的炒麦芽样品进行黄曲霉毒素污染状况调查;模拟炒麦芽的茶汤制备过程,考察黄曲霉毒素向茶汤中的迁移情况。结果炒麦芽中黄曲霉毒素的检出限和定量限分别为0.1~0.3µg/kg和0.4~0.8µg/kg,加标回收率在86.1%~111.2%之间,精密度为2.5%~7.0%。72个批次炒麦芽样品的黄曲霉毒素检出率为9.7%,阳性样品中4种黄曲霉毒素总量在2.7~22.3μg/kg之间。炒麦芽中黄曲霉毒素向茶汤中的迁移率在11.0%~17.0%之间。结论该方法准确、灵敏,适用于炒麦芽中黄曲霉毒素的测定;炒麦芽样品中黄曲霉毒素的检出率及其向茶汤中的迁移率总体较低。

Objective To determine aflatoxin B1,B2,G1,and G2 in processed Hordei Fructus Germinatus by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),and investigate the situation and their transfer rates from processed Hordei Fructus Germinatus to tea.Methods The content of aflatoxinss B1,B2,G1,and G2 in processed Hordei Fructus Germinatus were determined by HPLC-MS/MS,using 13 C-stable isotope labeled aflatoxins as internal standards and immunoaffinity column for sample cleanup,and the method was validated.A total of 72 samples of processed Hordei Fructus Germinatus were screened for aflatoxins contamination.The preparation process of tea with processed Hordei Fructus Germinatus was simulated to investigate the transfer of aflatoxins into the tea.Results The limits of detection and limits of quantitation of aflatoxins in processed Hordei Fructus Germinatus were 0.1-0.3μg/kg and 0.4-0.8μg/kg,respectively.The recoveries were in the range of 86.1%-111.2%with the precisions of 2.5%-7.0%.The detection rate of aflatoxins in 72 batches of processed Hordei Fructus Germinatus samples was 9.7%,and the total amount of 4 kinds of aflatoxins in positive samples ranged from 2.7 to 22.3μg/kg.The transfer rates of aflatoxins from processed Hordei Fructus Germinatus to tea was between 11.0%and 17.0%.Conclusion This method is accurate,sensitive and suitable for the determination of aflatoxins in processed Hordei Fructus Germinatus.The detection rates of aflatoxins in processed Hordei Fructus Germinatus samples and their transfer rates to tea were generally low.