生物胺是一类有毒有害的含氮化合物,存在于发酵食品中。目前检测生物胺的方法存在前处理复杂繁琐、耗时长等问题。该文通过实时直接分析离子源与三重四极杆质谱联用技术建立快速检测白酒中生物胺的外标定量方法,对实时直接分析(direct analysis in real time, DART)参数、进样速度、采样模式和溶剂进行优化,测定的生物胺包括腐胺(putrescine, PUT)、组胺(histamine, HIS)、尸胺(cadaverine, CAD)、酪胺(tyramine, TYR)和色胺(tryptamine, TRP)。结果表明,400 ℃为DART源的最优工作温度,进样速度为1 mm/s时,生物胺色谱峰峰形尖锐且峰间距适宜。使用Quick Strip采样模式分析物的相对标准偏差低于20%,生物胺回归系数(R2)大于0.99,方法检出限为8.60~38.00 μg/L,定量限为28.75~126.50 μg/L。该方法是一种现场、无损、快速、低碳、原位、直接分析的方法,适用于白酒中生物胺的快速筛查评估,操作上极大地满足了白酒行业对质量安全控制和风险评估的需求。
Biogenic amines are toxic and harmful nitrogenous compounds found in fermented foods.The current methods for the detection of biogenic amines are complicated and time-consuming.In this paper, an external standard quantitative method for the rapid determination of biogenic amines in Baijiu was established by direct analysis in real-time coupled with triple quadrupole mass spectrometry (DART-QQQ), and the parameters of direct analysis in real-time (DART), injection speed, sampling mode, and solvent were optimized.The biogenic amines determined included putrescine (PUT), histamine (HIS), cadaverine (CAD), tyramine (TYR), and tryptamine (TRP).Results showed that 400 ℃ was the optimal working temperature for the DART source, the peak shape of the biogenic amine peaks was sharp, and the peak spacing was suitable at an injection rate of 1 mm/s.The relative standard deviations (RSDs) of the analytes using Quick Strip sampling mode were lower than 20%, the regression coefficients (R2) of biogenic amines were greater than 0.99, the limits of detection (LODs) of the method were in the range of 8.60-38.00 μg/L, and the limits of quantification (LOQs) of the method were in the range of 28.75-126.50 μg/L.In conclusion, the method was an on-site, non-destructive, rapid, low-carbon, in situ, direct analysis method for the rapid screening and assessment of biogenic amines in Baijiu, and the operation greatly met the needs of the Baijiu industry for quality and safety control and risk assessment.
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