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.
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(ESI)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.
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
轻工业
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
ultra-high performance liquid chromatography-tandem mass spectrometry;fumonisins;mycotoxin;infant food;milk powder;milk
《乳业科学与技术》 2023 (006)
34-39 / 6
内蒙古自治区重点研发和成果转化计划项目(2023YFHH0093)
10.7506/rykxyjs1671-5187-20231201-058
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