食品科学 ›› 2017, Vol. 38 ›› Issue (12): 286-291.doi: 10.7506/spkx1002-6630-201712044

• 安全检测 • 上一篇    下一篇

HPLC法测定渝东南地区传统土家特色酸鲊肉中的组胺含量

冉春霞,陈光静,胡江   

  1. 1.重庆三峡医药高等专科学校医学技术系,重庆 404120;2.重庆市抗肿瘤天然药物工程技术研究中心,重庆 404120;3.西南大学食品科学学院,重庆 400715;4.重庆市万州区农产品质量安全监督检测中心,重庆 404120
  • 出版日期:2017-06-25 发布日期:2017-06-26
  • 基金资助:
    重庆市教委科学技术研究项目(KJ1502608)

Determination of Histamine Content in Suanzharou, a Unique and Traditional Fermented Meat Product of the Tujia Nationality in Southeastern Chongqing by High Performance Liquid Chromatography

RAN Chunxia, CHEN Guangjing, HU Jiang   

  1. 1. Department of Medical Technology, Chongqing Three Gorges Medical College, Chongqing 404120, China; 2. Chongqing Engineering Research Center of Antitumor Natural Drugs, Chongqing 404120, China; 3. School of Food Science, Univerisity of Southwest, Chongqing 400715, China; 4. Chongqing District of Wanzhou City Agricultural Products Quality Safety Supervision and Inspection Center, Chongqing 404120, China
  • Online:2017-06-25 Published:2017-06-26

摘要: 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?C18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。

关键词: 渝东南地区, 传统土家特色酸鲊肉, 组胺, 高效液相色谱法

Abstract: The purpose of this study was to establish a high performance liquid chromatography (HPLC) method for the qualitative and quantitative detection of histamine in Suanzharou, a unique and traditional fermented meat product of the Tujia nationality in southeastern Chongqing. 1,7-Heptanediamine was used as an internal standard substance. Dansyl chloride was used as a derivatization agent. The chromatographic separation was accomplished using an Agilent C18 column as stationary phase and a mixture of 70% methanol and 30% ultra pure water as mobile phase, and the UV detector was set at 254 nm. The analyte was extracted with 0.4 mol/L HClO4 solution and analyzed by HPLC. Results showed that the peaks for 1,7-heptanediamine and histamine dihydrochloride appeared at 4.335 min and 7.723 min, respectively, and an acceptable separation was achieved. The proposed method showed a good linearity between the ratio of peak area (histamine dihydrochloride and 1,7-heptanediamine) and the mass concentration of histamine. The recovery of spiked samples was between 98.5%–102.2%, the instrumental limit of detection (LOD) was 0.50 mg/L and the limit of quantitation (LOQ) was 1.00 mg/L. The precision expressed as relative standard deviation (RSD) was 1.0%. The histamine content of 10 real samples was detected to be in the range of 19.68–44.15 mg/kg, with significant differences existing among these samples (P < 0.05). In conclusion, this method is reliable for the detection of histamine in Suanzharou with high sensitivity and precision.

Key words: southeastern Chongqing, Suanzharou, histamine, HPLC

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