三重四级杆液质法检测食品中毒黄素和米酵菌酸含量  

Toxoflavin and Bongkrekic Acid in Foods:Determination by UPLC-MS/MS with Triple Quadrupole

作　　者：赵智锋 王晓琴 叶文芳 车宇慧 黄秀丽 陈榕德 甘维明 陈嘉聪 ZHAO Zhifeng;WANG Xiaoqin;YE Wenfang;CHE Yuhui;HUANG Xiuli;CHEN Rongde;GAN Weiming;CHEN Jiacong(Huizhou Institute for Food and Drug Control,Huizhou,Guangdong 516000;Shenzhen Xince Standard Technical Service Co.,Ltd.,Shenzhen,Guangdong 518000)

机构地区：[1]惠州市食品药品检验所,广东惠州516000 [2]深圳信测标准技术服务股份有限公司,广东深圳518000

出　　处：《中国农学通报》2024年第3期128-134,共7页Chinese Agricultural Science Bulletin

基　　金：惠州市科技计划社会发展领域项目“椰毒假单胞菌酵米面亚种长度机制及关键控制技术研究”(2021WC010301);惠州市科技计划社会发展领域项目“椰毒假单胞菌酵米面亚种毒素一测多评及控制关键技术研究”(2020SC0204013)。

摘　　要：旨在建立利用三重四级杆液相色谱质谱(UPLC-MS/MS)同时测定食品中毒黄素和米酵菌酸含量的方法。样品在80%甲醇水溶液体系中萃取,离心后上清液经QuEChERS EMR-Lipid净化处理,浓缩、复溶后,以0.1%甲酸水和乙腈为流动相经梯度洗脱,液质电喷雾离子源正负模式检测,使用外标法进行定量分析。实验结果显示,毒黄素和米酵菌酸在浓度为0.5~100μg/L的范围内表现出较好线性关系,线性线性相关系数r大于0.995,在不同基质多水平添加浓度下,回收率为86.8%~103.6%,相对标准偏差(RSD)小于5%,毒黄素方法检出限为0.1μg/kg,定量限为0.2μg/kg,米酵菌酸方法检出限为0.05μg/kg,定量限为0.1μg/kg。该方法灵敏度高、专属性好、准确可靠,适合食品中毒黄素和米酵菌酸含量的测定。The contents of toxoflavin(TF)and bongkrekic acid(BA)in foods are determined simultaneously by an ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method.The samples were ultrasonically extracted with 80%methanol aqueous solution.After centrifugation,the supernatants were purified by the QuEChERS EMR-Lipid.And after concentration and reconstitution,the samples were eluted by gradient with 0.1%formic acid solution water and acetonitrile as mobile phases,which was detected by liquid-mass electrospray ion source in positive and negative modes,and quantified by external standard method.The results indicated that the TF and BA showed good linearity in the concentration range of 0.5-100μg/L,and the correlation coefficient was larger than 0.995.Under different additive concentrations of various substrates,the recoveries were 86.8%-103.6%,and the average relative standard deviations(RSD)were less than 5%.The detection limit of the TF method was 0.1μg/kg and the quantification limit was 0.2μg/kg.Meanwhile,the detection limit of the BA method was 0.05μg/kg,and the quantification limit was 0.1μg/kg.The method has high sensitivity,good specificity,accuracy and reliability,and is suitable for the determination of TF and BA in foods.

关 键 词：毒黄素 米酵菌酸 三重四级杆液质法 QUECHERS 

分 类 号：S-3[农业科学]