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三重四级杆液质法检测食品中毒黄素和米酵菌酸含量

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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0.1 μg/kg,定量限为0.2 μg/kg,米酵菌酸方法检出限为0.05 μg/kg,定量限为0.1 μg/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.
Toxoflavin and Bongkrekic Acid in Foods:Determination by UPLC-MS/MS with Triple Quadrupole
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 0.5-100 μg/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 0.1 μg/kg and the quantification limit was 0.2 μg/kg.Meanwhile,the detection limit of the BA method was 0.05 μg/kg,and the quantification limit was 0.1 μg/kg.The method has high sensitivity,good specificity,accuracy and reliability,and is suitable for the determination of TF and BA in foods.

toxoflavinbongkrekic acidultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)with triple quadrupoleQuEChER

赵智锋、王晓琴、叶文芳、车宇慧、黄秀丽、陈榕德、甘维明、陈嘉聪

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惠州市食品药品检验所,广东惠州 516000

深圳信测标准技术服务股份有限公司,广东深圳 518000

毒黄素 米酵菌酸 三重四级杆液质法 QuEChERS

惠州市科技计划社会发展领域项目惠州市科技计划社会发展领域项目

2021WC0103012020SC0204013

2024

中国农学通报
中国农学会

中国农学通报

CSTPCD
影响因子:0.891
ISSN:1000-6850
年,卷(期):2024.40(3)
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