液相色谱串联质谱法测定传统豆制品白豆干和薄百叶中的生物胺

Detection of biogenic amines of traditional soybean products using high performance liquid chromatography-mass spectrometry/mass spectrometry

建立了传统豆制品白干和薄百叶中六种生物胺的高效液相色谱串联质谱法的测定方法。样品以三氯乙酸提取，经混合型阳离子交换固相萃取小柱净化后进样分析。采用AtlantisHILIC色谱柱（150．0mm×2．1mm，3μm），乙腈与水（含2mmol／L乙酸铵，0．1％甲酸）梯度进样，采用电喷雾离子源正离子模式，多反应监测（MRM）模式，外标法进行质谱定量分析，分析时间为15min。本方法在0～1000μg／kg范围内呈良好的线性关系（r〉0．991）；六种生物胺混合标准溶液中加标量为100μg／kg，检出限（LOD）为10～50txg／kg，定量限为33．3～166．6μg／kg；平均添加回收率为72．5％～108．2％，标准偏差为6．2％～13.2％。本方法具有操作简便、快速、准确、灵敏度高等优点，适用于多种生物胺的同时定性与定量分析，为豆制品中生物胺的进一步研究提供了有效且便利的分析方法。

A confirmative method was developed to detect 6 biogenic amines in traditional soybean products by HPLC-MS/MS. Biogenic amines were extracted with acetocaustin. The separation of biogenic amines were carried out based on Sunfire Atlantis HILIC column（150.0mm×2.1mm,3μm）,with a gradient elution of acetonitrile and water（including 2mmol/L ammonium acetate,0.1% formic acid）. The detection method of electrospray ionization source with positive-ion electrospray ionization mode was used for mass spectrometric analysis. Qualitative and quantitative analysis of the 6 biogenic amines were completed within 15min. Experimental results showed that the biogenic amines had a good linearity（r〉0.991 ） in the range of 0~1000tJg/kg. The limit of detection （LOD） was 10~50μg/kg. The limits of quantification were 33.3-166.6μg/kg. The average recoveries were 72.5%-108.2%. The relative standard deviations were 6.2%-13.2%. The results showed that it was a simple,rapid,accurate and highly sensitive method to analyze and detect the biogenic amines in the traditional soybean products.