超高效液相色谱-串联质谱法测定牛乳和乳粉中伏马毒素残留

doi:10.7506/rykxyjs1671-5187-20231201-058

乳业科学与技术 ›› 2023, Vol. 46 ›› Issue (6): 34-39.DOI: 10.7506/rykxyjs1671-5187-20231201-058

超高效液相色谱-串联质谱法测定牛乳和乳粉中伏马毒素残留

莫楠，张立佳，高玉杰，白艳梅，汪洋，刘丽君，李翠枝

内蒙古伊利实业集团股份有限公司，内蒙古呼和浩特 010110

发布日期:2024-03-27
基金资助:
内蒙古自治区重点研发和成果转化计划项目（2023YFHH0093）

Quantitative Determination of Fumonisin Residues in Milk and Milk Powder by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

MO Nan, ZHANG Lijia, GAO Yujie, BAI Yanmei, WANG Yang, LIU Lijun, LI Cuizhi

Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 010110, China

Online:2024-03-27

摘要/Abstract

摘要： 建立在乳粉、牛乳2 种基质中超高效液相色谱-串联质谱法同时检测伏马毒素B1（fumonisin B1，FB1）、FB2和FB3残留的检测方法。样品以体积分数50%乙腈溶液提取，稀释后经免疫亲和柱净化，甲醇-乙酸（98∶2，V/V）洗脱，氮吹后复溶，采用电喷雾离子源正离子多反应监测模式进行检测，同位素内标法定量。结果表明：本方法牛乳、乳粉基质中FB1、FB2和FB3定量限均为10 μg/kg，药物加标量10～400 μg/kg时，加标回收率为92.8%～107.5%，相对标准偏差为2.0%～4.3%，基质效应为96.25%～122.84%。该方法具有检测周期短、适用于多种婴幼儿食品检测的特点。

关键词: 超高效液相色谱-串联质谱；伏马毒素类；真菌毒素；婴幼儿食品；乳粉；牛乳

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous quantitative determination of fumonisin B1 (FB1), fumonisin B2 (FB2) and fumonisin B3 (FB3) residues in milk powder and milk has been established. The samples were extracted with methanol-acetic acid (98:2, V/V), diluted, cleaned up by immunoaffinity chromatography (IAC), and blown to dryness under nitrogen. The residue was re-dissolved and detected using an electrospray ionization source (EIS) in the positive ion mode with multiple reaction monitoring (MRM) and quantitative analysis was performed by the isotope-labeled internal standard method. The limit of quantification was 10 μg/kg for FB1, FB2 and FB3 in milk powder and milk. The recoveries at spiked concentration levels of 10–400 μg/kg were 92.8%–107.5%, with relative standard deviations (RSD) of 2.0%–4.3%. The matrix effects were 96.25%–122.84%. This method was characterized by short analysis time and was suitable for the determination of fumonisin residues in different dairy products.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; fumonisins; mycotoxin; infant food; milk powder; milk

中图分类号:

TS252.7

莫楠，张立佳，高玉杰，白艳梅，汪洋，刘丽君，李翠枝. 超高效液相色谱-串联质谱法测定牛乳和乳粉中伏马毒素残留[J]. 乳业科学与技术, 2023, 46(6): 34-39.

MO Nan, ZHANG Lijia, GAO Yujie, BAI Yanmei, WANG Yang, LIU Lijun, LI Cuizhi. Quantitative Determination of Fumonisin Residues in Milk and Milk Powder by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Dairy Science and Technology, 2023, 46(6): 34-39.

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超高效液相色谱-串联质谱法测定牛乳和乳粉中伏马毒素残留

Quantitative Determination of Fumonisin Residues in Milk and Milk Powder by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

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