复合柱净化-超高效液相色谱-串联质谱法测定粮油中黄曲霉毒素和玉米赤霉烯酮类毒素  

Determination of aflatoxins and zearalenone in vegetable oil and cereal products by solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry

作　　者：宋月[1] 杨丽君[1] 吴平谷[2] 康译友[1] SONG Yue;YANG Lijun;WU Pinggu;KANG Yiyou(Dalian Municipal Center for Disease Control and Prevention,Liaoning Dalian 116021,China;Zhejiang Provincial Center for Disease Control and Prevention,Zhejiang Hangzhou 310051,China)

机构地区：[1]大连市疾病预防控制中心,辽宁大连116021 [2]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国食品卫生杂志》2020年第1期39-44,共6页Chinese Journal of Food Hygiene

基　　金：大连市医学科学研究计划项目(1811098).

摘　　要：目的建立C18-Al2O3复合固相萃取柱净化,同时检测粮食及植物油中黄曲霉毒素和玉米赤霉烯酮类毒素的超高效液相色谱-串联质谱方法。方法植物油样品用乙腈-水(90∶10,V∶V)提取,粮食样品先用乙腈-乙酸-水(84∶1∶16,V∶V)再用二氯甲烷-乙酸乙酯(90∶10,V∶V)进行二次提取,进一步采用C18-Al2O3复合固相萃取柱净化,稳定同位素内标稀释,以乙腈和水为流动相,CORTECSTMC18色谱柱(2.1 mm×100 mm,2.7μm)进行分离,电喷雾离子化多反应监测模式检测。结果黄曲霉毒素和玉米赤霉烯酮类毒素的线性范围分别为0.1~30.0和1.0~500.0ng/ml,检出限分别为0.03和0.3μg/kg,定量限分别为0.10和1.0μg/kg。黄曲霉毒素和玉米赤霉烯酮类毒素的平均回收率分别为68.3%~98.6%和84.5%~108.0%,相对标准偏差分别为4.6%~11.5%和4.2%~9.0%(n=6)。采用本方法分析了国内外5种质控样品,测定值均在质控样品指定范围内。对大连市市售的100份粮油样品进行测定,结果表明散装花生油和玉米油中黄曲霉毒素B1和玉米赤霉烯酮检出率较高,最高含量分别为12.80和370.00μg/kg。结论本方法定量准确、操作简便、更环保、检测成本低,适于批量粮油样品中黄曲霉毒素和玉米赤霉烯酮类毒素的同时检测。Objective To develop a method for simultaneous determination of aflatoxins(AFs)and zearalenone(ZEN)in vegetable oil and cereal products by solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC).Methods AFs and ZEN in vegetable oil were extracted by acetonitrile-water solution(90∶10,V∶V).AFs and ZEN in cereals were firstly extracted by acetonitrile-acetic acidwater solution(84∶1∶16,V∶V)and then extracted by dichloromethane/ethyl acetate(90∶10,V∶V),and the extracts were concentrated and reconstructed by acetonitrile-water solution(90∶10,V∶V).The extracts of vegetable oil/cereals were purified by C18-Al2O3 solid phase extraction column.AFs and ZEN were separated by UPLC with acetonitrile-water gradient elution in a CORTECSTMC18 chromatography column(2.1 mm×100 mm,2.7μm),and qualified/quantified by mass spectrometry with electron spray ionization multiple reaction monitoring mode with stableisotope internal standard.Results The linearity of AFs and ZEN were 0.1-30.0 and 1.0-500.0 ng/ml,the limits of detection were 0.03 and 0.3μg/kg,and the limits of quantification were 0.10 and 1.0μg/kg,respectively.The average recoveries of AFs and ZEN for spiked samples was 68.3%-98.6%and 84.5%-108.0%with the relative standard deviation4.6%-11.5%and 4.2%-9.0%(n=6),respectively.Several quality control material were analyzed to verified the accuracy of the method.100 samples sold in Dalian markets were analyzed.Aflatoxin B1 and ZEN was detected in peanut oil and corn oil samples with maximum contents 12.80 and 370.00μg/kg,respectively.Conclusion The method had several advantages including accurate,simple and cost-effective,environment friendly and it was applicable to batch analysis of AF and ZEN in vegetable oil and cereal products.

关 键 词：黄曲霉毒素 玉米赤霉烯酮 α-玉米赤霉烯醇 真菌毒素 固相萃取 超高效液相色谱-串联质谱 玉米油 花生油 

分 类 号：O657.63[理学—分析化学] TS207.4[理学—化学]