Todoroki Kenichiro, Ishii Yasuhiro, Miyauchi Chiemi, Kitagawa Sachiyo, Min Jun Zhe, Inoue Koichi, Yamanaka Tomoyuki, Suzuki Kuniaki, Yoshikawa Yuko, Ohashi Norio, Toyo'oka Toshimasa
Laboratory of Analytical and Bio-Analytical Chemistry, School of Pharmaceutical Sciences, University of Shizuoka , 52-1 Yada, Suruga, Shizuoka 422-8526, Japan.
J Agric Food Chem. 2014 Jul 2;62(26):6206-11. doi: 10.1021/jf500767p. Epub 2014 Jun 18.
We established a simple, sensitive, and reproducible method to analyze the histamine and tyramine levels in Japanese soy sauce and its mash (called moromi) using hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS). Histamine and tyramine quantification was performed using their stable isotopes for electrospray ionization-tandem mass spectrometry in the selected reaction monitoring mode. The sample pretreatment process was a simple, one-step liquid-liquid extraction. HILIC separation was performed with a gradient elution of aqueous ammonium formate and acetonitrile. Because of validation tests, the linearity, the accuracies, and precisions were sufficient. The limit of detection and the limit of quantification were 0.09 and 0.29 ppm for histamine and 0.13 and 0.42 ppm for tyramine, respectively. We successfully applied this method to histamine and tyramine determination in four kinds of commercial Japanese soy sauces and also in moromi samples during soy sauce production.
我们建立了一种简单、灵敏且可重复的方法，使用亲水作用液相色谱-串联质谱法（HILIC-MS/MS）分析日本酱油及其酱醪（称为“醪”）中的组胺和酪胺水平。组胺和酪胺的定量分析采用其稳定同位素，在选择反应监测模式下进行电喷雾电离-串联质谱分析。样品预处理过程是简单的一步液-液萃取。采用甲酸铵水溶液和乙腈梯度洗脱进行亲水作用液相色谱分离。经过验证测试，线性、准确度和精密度均足够。组胺的检测限和定量限分别为0.09 ppm和0.29 ppm，酪胺的检测限和定量限分别为0.13 ppm和0.42 ppm。我们成功地将该方法应用于四种市售日本酱油以及酱油生产过程中醪样品中组胺和酪胺的测定。
