免疫亲和柱净化-液相色谱-串联质谱法测定广式月饼中的伏马毒素B_1、B_2

Determination of fumonisin B_1 and B_2 in Cantonese moon cake by liquid chromatography- tandem mass spectrometry with immunoaffinity purification

目的建立广式月饼中的伏马毒素(FB_1、FB_2)定性和定量的液相色谱-串联质谱法。方法广式月饼样品经甲醇-水(8∶2,V/V)溶液均质提取后,用免疫亲和柱净化,经PBS洗脱,以乙酸铵溶液(5 mmol/L,p H=4.5)和乙腈为流动相,流速为400μl/min,柱温为30℃,在C18色谱柱上梯度洗脱分离,采用电喷雾正离子多反应监测(MRM)模式测定。结果 FB_1、FB_2的质量浓度为0.1 ng/ml^50.0 ng/ml时,标准曲线的线性关系良好;用本法测定的2种伏马毒素的回收率为79.2%~102.3%,相对标准偏差(RSD)为3.6%~8.7%。采用该方法对市售的5种广式月饼中的伏马毒素进行分析,其中1份广式月饼样品能够检测到含有痕量的FB1(0.56μg/kg)和FB2(0.73μg/kg)。结论该方法具有简单、快速、准确、可靠等特点,适用于广式月饼中2种伏马毒素的同时测定。

Objective To develop a method for the identification and quantification determination of fumonisin B1 and fumonisin B2 in Cantonese moon paste cake using liquid chromatography- tandem mass spectrometry（ LC- MS / MS）. Methods The sample was extracted with methanol- water（ 8 ∶2,V / V） solution,followed by a cleanup procedure with immunoaffinity column,and then eluted by PBS. FB1 and FB2were separated on a C18 column using acetonitrile and ammonium acetate solution（ 5 mmol/L,p H = 4. 5） as mobile phase at a constant temperature of 30 ℃ and at a flow rate of 400 μl/min,and then detected in positive ion mode with multiple reaction monitoring（ MRM）. Results With the concentration of FB1 and FB2among 0. 1 ng / ml-50. 0 ng / ml,the linear relationship of standard curve was good; the recovery rates for FB1 and FB2were among 79. 2%-102. 3% with this method for detection,while the relative standard deviations（ RSD） was among 3. 6%- 8. 7%. Little amounts of FB1（ 0. 56 μg/kg） and FB2（ 0. 73 μg/kg） were detected in one of five moon paste cakes using this method. Conclusion The developed method is simple,fast,accurate,reliable,and can be applied for the simultaneous determination of FB1 and FB2in Cantonese moon paste cake.