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中国农学通报

中国农学通报 ›› 2024, Vol. 40 ›› Issue (3): 128-134.doi: 10.11924/j.issn.1000-6850.casb2022-0451

• 食品·营养·检测·安全 • 上一篇    下一篇

三重四级杆液质法检测食品中毒黄素和米酵菌酸含量

赵智锋1(), 王晓琴1, 叶文芳1, 车宇慧1, 黄秀丽1, 陈榕德1, 甘维明2, 陈嘉聪1()   

  1. 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
  • 收稿日期:2022-06-25 修回日期:2022-08-15 出版日期:2024-01-17 发布日期:2024-01-17
  • 通讯作者:
    陈嘉聪，男，1982年出生，广东惠州人，高级工程师，本科，研究方向：食品检测技术。通信地址：516003 广东省惠州市惠城区江北文成路13号3楼，质量管理室，Tel：0752-2840402，E-mail：。
  • 作者简介:

    赵智锋，男，1980年出生，广东惠州人，高级工程师，本科，研究方向：食品安全与检测。通信地址：516003 广东省惠州市惠城区江北文成路13号7楼，食品检验室，Tel：0752-2840370，E-mail：。

  • 基金资助:
    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)

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

ZHAO Zhifeng1(), WANG Xiaoqin1, YE Wenfang1, CHE Yuhui1, HUANG Xiuli1, CHEN Rongde1, GAN Weiming2, CHEN Jiacong1()   

  1. 1 Huizhou Institute for Food and Drug Control, Huizhou, Guangdong 516000
    2 Shenzhen Xince Standard Technical Service Co., Ltd., Shenzhen, Guangdong 518000
  • Received:2022-06-25 Revised:2022-08-15 Published-:2024-01-17 Online:2024-01-17

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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0.5~100 μg/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。

关键词: 毒黄素, 米酵菌酸, 三重四级杆液质法, QuEChERS

Abstract:

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.

Key words: toxoflavin, bongkrekic acid, ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) with triple quadrupole, QuEChER