高效液相色谱-荧光法检测咖啡及其制品中3种赭曲霉毒素  

Determination of Three Ochratoxins in Coffee and its Products by High Performance Liquid Chromatography with Fluorescence Detection

作　　者：张迎周 李艳美 史华进 李芳 李庆 樊定艳 陈曦 ZHANG Ying-zhou;LI Yan-mei;SHI Hua-jin;LI Fang;LI Qing;FAN Ding-yan;CHEN Xi(GRA(Shanghai)Standard Technology Service Co.,Ltd.,Shanghai 201318,China;Yining Customs Technology Center,Yining 835000,China;Thermo Fisher Scientific(China)Co.,Ltd.,Shanghai 201206,China)

机构地区：[1]普研(上海)标准技术服务有限公司,上海201318 [2]伊宁海关技术中心,新疆伊宁835000 [3]赛默飞世尔科技(中国)有限公司,上海201206

出　　处：《化学试剂》2025年第2期79-84,共6页Chemical Reagents

基　　金：新疆维吾尔自治区自然科学基金项目(2021D01A188)。

摘　　要：通过前处理和液相色谱条件的优化,建立高效液相色谱-荧光检测咖啡及其制品中赭曲霉毒素A、赭曲霉毒素B和赭曲霉毒素C含量的方法。样品经过V(1%碳酸氢钠水溶液)∶V(乙腈)=40∶60提取,赭曲霉毒素A免疫亲和柱富集净化,以2%乙酸水溶液-乙腈为流动相,采用梯度洗脱方式在C 18色谱柱分离,荧光检测法对3种赭曲霉毒素进行定性和定量分析。结果表明:赭曲霉毒素在0.1~10.0μg/L浓度范围内呈现良好的线性关系(R 2>0.999),方法检出限均为0.1μg/kg,定量限均为0.3μg/kg,加标平均回收率为88.6%~95.0%,相对标准偏差为1.71%~3.15%。方法操作简单、灵敏度高、重现性好,适用于咖啡及其制品中赭曲霉毒素A、赭曲霉毒素B、赭曲霉毒素C含量的测定。A method for determining the content of ochratoxin A,ochratoxin B,and ochratoxin C in coffee and its products was established using high performance liquid chromatography-fluorescence detection.This method involved optimizing the pre-treatment and liquid chromatography conditions.The ochratoxins were extracted using V(1%sodium bicarbonate)∶V(acetonitrile)=40∶60 and then enriched and purified using ochratoxin A immunoaffinity column.The separation was achieved using a C 18 chromatography column with a gradient elution consisting of 2%acetic acid aqueous solution-acetonitrile as the mobile phase.Three ochratoxins were analyzed using fluorescence detection.The results demonstrated a good linear relationship among three ochratoxins within 0.1~10.0μg/L,with R 2>0.999.The limits of detection and the limits of quantification were 0.1 and 0.3μg/kg,respectively.The average recovery rate of spiked samples ranged from 88.6%to 95.0%,and the relative standard deviation was in the range of 1.71%~3.15%.This method is simple,highly sensitive,and exhibits good reproducibility,making it suitable for the determination of ochratoxin A,ochratoxin B,and ochratoxin C in coffee and its products.

关 键 词：高效液相色谱 赭曲霉毒素A 赭曲霉毒素B 赭曲霉毒素C 咖啡 

分 类 号：O65[理学—分析化学]