Abstract: A ultra performance liquid chromatography-tandem mass spectrometry(ultra-high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS) method for simultaneously quantitative determination of three kinds of (Fumonisin B1，FB1）, (Fumonisin B2，FB2） and (Fumonisin B3，FB3）residues in products, including milk powder and milk has been established. The samples were extracted with 5% formic acid acetonitrile. The samples were extracted with acetonitrile-water（1:1，V/V），diluted and cleaned up by IAC-SEP. After the residues of targets were eluted by methanol - acetic acid（98:2，V/V）, the elution was dried under nitrogen and then redissolved. The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring (MRM) mode and Quantitative analysis by isotope internal standard method. The limit of quantifification 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 2.4~4.3 %. The matrix effects were96.25~122.84%. 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

摘要： 建立在乳粉、牛乳2 种基质制品中超高效液相色谱-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。样品以乙腈-水溶液（1︰1，V/V）提取，经稀释后过免疫亲和柱净化，甲醇-乙酸溶液（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，药物添加范围10～400 μg/kg时，回收率为92.8%～107.5%之间，相对标准偏差为2.4%～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