液质联用法在火锅底料中黄曲霉毒素和赭曲霉毒素污染分析的应用
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作者单位:

浙江省疾病预防控制中心,理化与毒理检验所,浙江 杭州 310051

作者简介:

许娇娇 女 副主任技师 研究方向为食品污染物分析 E-mail:jjxucdc@163.com

通讯作者:

徐小民 男 主任技师 研究方向为食品污染物分析 E-mail:xmxu@cdc.zj.cn

中图分类号:

R155

基金项目:

浙江省基础公益研究计划(LTGC23H260001)


Application of ultra-performance liquid chromatography tandem mass spectrometry in analysis of aflatoxins and ochratoxin A in hotpot seasoning
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Institute of Physico-chemical and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang Hangzhou 310051, China

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    摘要:

    目的 建立并优化了火锅底料中黄曲霉毒素B族、G族和赭曲霉毒素A等5种真菌毒素的超高效液相色谱串联质谱检测方法,为火锅底料产品质量监管和风险预警提供技术支持。方法 样品用84%?乙腈-水提取后,经二合一真菌毒素免疫亲和柱净化,采用BEH C18(100 mm×2.1 mm,1.7 μm)进行分离,以0.1%甲酸溶液和乙腈-甲醇为流动相梯度洗脱,内标法定量。应用优化建立的液质联用法分析25份火锅底料产品中真菌毒素污染情况。结果 该方法在线性范围内0.1~20 ng/mL线性良好,火锅底料中黄曲霉毒素和赭曲霉毒素的方法检出限为0.03 μg/kg,定量限为0.1 μg/kg,加标回收率为90.59%~117.36%,RSD%为2.83%~9.44%。检测的25份火锅底料中,以黄曲霉毒素B1和赭曲霉毒素A为主要检出毒素,检出率分别为40%、72%。结论 本研究优化后的二合一免疫亲和柱净化的前处理方法针对性强,具有良好的灵敏度、加标回收率和精密度,适用于火锅底料中真菌毒素的定量分析,可为火锅底料中真菌毒素的风险监管和预警提供技术支持。

    Abstract:

    Objective To provide the technical support for hot pot base product supervision and risk warning, an ultra-high performance liquid chromatography-tandem mass spectrometry method for the detection of aflatoxins B group, G group and ochratoxin A in hotpot seasoning was established and optimized.Methods After extracted by 84% acetonitrile-water and cleaned up by 2 in 1 immunity column, 5 types target mycotoxins were separated by BEH C18(100 mm×2.1 mm,1.7 μm) under 0.1% formic acid and acetonitrile-methanol mobile phase. The optimized LC-MS/MS was validated and applicated in 25 hotpot seasoning samples from Internet merchant,which quantificated by internal standards.Results The method was validated and demonstrated a good linear relationship in range of 0.1-20 ng/mL. The detective limits were 0.03 μg/kg and the quantitative limits were 0.1 μg/kg. The recoveries were between 90.59% and 117.36%. The relative standard deviation were from 2.83% to 9.44%. The optimized method was applicated in 25 hotpot seasoning analysis, with detection rates of aflatoxin B1 and ochratoxin A 40% and 72%, respectively.Conclusion The optimized 2 in 1 immunoaffinity clean-up pretreatment in this study is highly targeted. The method has a good sensitivity, satisfied recovery rate and precision. It is suitable for the quantitative analysis of mycotoxins in hotpot seasoning, which could provide technical support for risk monitoring and early warning of mycotoxins in in hotpot seasoning.

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许娇娇,王梦莉,蔡增轩,黄百芬,徐小民.液质联用法在火锅底料中黄曲霉毒素和赭曲霉毒素污染分析的应用[J].中国食品卫生杂志,2025,37(1):36-41.

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  • 收稿日期:2024-06-17
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  • 在线发布日期: 2025-05-16
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