摘要
建立复合免疫亲和柱净化、超高效液相色谱串联质谱检测发酵豆制品中的黄曲霉毒素B1(AFB1)、赭曲霉毒素A(OTA)的新方法。样品经80%甲醇/水提取,去除油脂,提取液经复合免疫亲和柱净化浓缩后,Agilent EC-C18色谱柱分离,ESI+多反应监测,以内标法定量分析。结果表明AFB1的线性范围在0.02~5.0μg/L,相关系数(r)为0.9995,检出限为0.04μg/kg,定量限为0.15μg/kg。3加标水平下(0.2、0.8、5.0μg/kg)的回收率在88.2%~91.5%之间,相对标准偏差为5.0%~6.3%。OTA的线性范围在0.1~30.0μg/L,相关系数(r)为0.9995,检出限为0.2μg/kg,定量限为0.6μg/kg。3加标水平下(2、8、50μg/kg)的回收率在90.4%~94.5%之间,相对标准偏差为4.8%*6.1%。该方法快速准确,可用于发酵豆制品中AFB1和OTA的定性、定量检测。
A new method for determination of aflatoxins B1(AFB1)and ochratoxin A(OTA)in fermented soybean products using UPLC-MS/MS(Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry)with IAC(composite immunoaffinity column)was established.Samples were prepared by extracting with 80%methanol/water,degreasing and supernatant purification using immunoaffinity column.Chromatographic separation was achieved on an Agilent Eclipse Plus C18 chromatographic column;analytes were monitored using ESI-MRM,and quantified via an internal standard method.For AFB1,good linearity was obtained in a range of 0.02〜5.0μg/L,with the correlation coefficients(r)higher than 0.9995.The limit of detection(LOD)was 0.04μg/kg and the limit of quantitation(LOQ)was 0.15μg/kg.Average recoveries at three spiking levels(0.2,0.8,5.0μg/kg)ranged from 88.2%〜91.5%,with relative standard deviations of 5.0%〜6.3%.Similarly,OTAexhibited good linearity over the concentration range of 0.1〜30.0μg/L,with the correlation coefficients(r)higher than 0.9995,with an LOD of 0.2μg/kg and LOQ of 0.6μg/kg.Average recoveries at three spiking levels of 2,8,50μg/kg were in the range of 90.4%〜94.5%,with RSDs of 4.8%〜6.1%.The results showed that this developed method was rapid,accurate and suitable for qualitative and quantitative determination of AFB1 and OTA in fermented soybean products.
作者
平文卉
张璐璐
程晓宏
杨清华
杨娟
谢超
张茹月
PING Wenhui;ZHANG Lulu;CHENG Xiaohong;YANG Qinghua;YANG Juan;XIE Chao;ZHANG Ruyue(Nantong Center for Disease Control and Prevention,Nantong 226007)
出处
《中国食品添加剂》
2025年第9期151-155,共5页
China Food Additives
基金
南通市“十四五”医学重点学科
南通市“十四五”青年医学人才
江苏省卫健委课题(Z2024030)。
