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建立测定渝东南地区传统土家特色酸鲊肉中组胺含量的高效液相色谱(high performance liquid chromatography,HPLC)方法,并进行样品中组胺含量的测定。以1,7-庚二胺为内标物,丹磺酰氯为样品衍生剂;Agilent C_(18)柱为固定相,70%甲醇和30%超纯水为流动相,于波长254 nm处进行紫外检测。用0.4 mol/L高氯酸溶液提取样品中的组胺,然后测定酸鲊肉中的组胺含量。结果表明:内标物和组胺标准品分别在4.335 min和7.723 min出峰,且分离效果良好。经实验验证,组胺盐酸盐标准品的峰面积和内标物峰面积的比值与组胺质量浓度之间存在良好的线性关系,样品加标实验回收率在98.5%~102.2%之间;仪器检出限为0.50 mg/L,定量限为1.00 mg/L,精密度相对标准偏差为1.0%。经检测10个样品中组胺含量在19.68~44.15 mg/kg之间,不同样品组胺含量有显著性差异(P<0.05)。本研究表明HPLC方法的灵敏度和精密度较高,是检测酸鲊肉中组胺含量的可靠方法。
A high performance liquid chromatography (HPLC) method was established for the determination of histamine content in traditional Tujia sour pterygium in the southeastern region of Chongqing. The histamine content in the samples was determined. Dansyl chloride was used as the sample derivatization reagent with 1,7-heptanediamine as the internal standard. Agilent C_ (18) column was used as stationary phase. The mobile phase consisted of 70% methanol and 30% ultrapure water at a wavelength of 254 nm UV detection. Histamine in the sample was extracted with a 0.4 mol / L perchloric acid solution and the histamine content in sarcocarp was measured. The results showed that the internal standards and histamine standards peaked at 4.335 min and 7.723 min, respectively, and the separation effect was good. The experimental verification shows that there is a good linear relationship between the ratio of the peak area of the histamine hydrochloride standard and the peak area of the internal standard and the concentration of the histamine, and the recoveries of the spiked samples are between 98.5% and 102.2% The detection limit was 0.50 mg / L, the limit of quantification was 1.00 mg / L, and the relative standard deviation of precision was 1.0%. Histamine content of the 10 samples tested ranged from 19.68 to 44.15 mg / kg, and the histamine contents of different samples were significantly different (P <0.05). This study shows that the high sensitivity and precision of the HPLC method is a reliable method of detecting histamine content in sour pomfret.