直接稀释-UHPLC-MS/MS同时测定黄酒中的9种生物胺

目的 建立黄酒中组胺、酪胺、色胺、腐胺、尸胺、苯乙胺、章鱼胺、吡哆胺和1，6-己二胺的直接稀释-超高效液相色谱串联质谱（UHPLC-MS/MS）同时检测方法。方法 黄酒样品中加入内标1，7-二氨基庚烷并用0.10mol/L HCl稀释后，过0.22 μm微孔滤膜，采用RRHD HILIC Plus色谱柱（2.1mm×100mm，1.8μm）为分离柱、甲醇-8mmol/L乙酸铵水溶液为流动相，梯度洗脱分离；并用多反应监测模式检测、内标法定量。结果 9种生物胺在10~500ng/mL浓度范围内呈现良好线性（相关系数r>0.99）。方法检出限（LOD）为0.21~0.51ng/mL，定量限（LOQ）为0.68~1.71ng/mL；除章鱼胺外，其余8种生物胺的加标回收率为61.68%~129.5%，相对标准偏差为0.32%~6.15%。应用本法对市售黄酒样品中的生物胺进行了分析，均未检出章鱼胺和吡哆胺，2-苯乙胺、1，6-己二胺、酪胺、尸胺、组胺、色胺的含量在1.01~24.6μg/mL范围内。结论 所建立的 UHPLC-MS/MS检测法具有简便、快速、灵敏、准确的优点，可用于黄酒中生物胺的检测。

Simultaneous determination of 9 biogenic amines in rice wine by direct dilution-UHPLC-MS/MS

Objective To establish a direct dilution-ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) for simultaneous determination of nine biogenic amines (BAs) in rice wine, including histamine, tyramine, tryptamine, humidine, cadreamine, phenylethylamine, octopamine, pyridoxine and 1, 6-hexanediamine. WTHZ]Methods The rice wine samples were spiked with 1, 7-diaminoheptane (internal standard) and diluted with 0.10mol/L HCl solution, filtered by 0.22μm microporous membrane. The BAs in filtrate were separated by gradient elution on a RRHD HILIC Plus column (2.1mm×100mm, 1.8μm) with the mobile phase consisting of methanol-8 mmol/L ammonium acetate solution and detected by MS/MS in multiple reaction monitoring (MRM) mode. WTHZ]Results The nine biogenic amines showed good linearity in the range of 10-500 ng/mL (r>0.99). The detection limits (LODs) and the quantification limits (LOQs) of the proposed method were in the range of 0.21-0.51ng/mL and 0.68-1.71ng/mL, respectively. The spiked recoveries for BAs except octopamine ranged from 61.68% to 129.53%; the relative standard deviations were 0.32%-6.15%. This method had been applied to analysis of the commercial rice wine, and neither octopamine nor pyridoxamine was detected. The contents of 2-phenylethylamine, 1,6-hexanediamine, tyramine, cadaverine, histamine, and tryptamine were in the range of 1.01-24.6μg/mL. WTHZ]Conclusion The established UHPLC-MS/MS method is simple, fast, sensitive, and accurate, and it is suitable for the analysis of the nine BAs in rice wine.