食品科学

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黄酒中9 种生物胺的高效液相色谱分析法

曹利瑞1,朱 松2,俞剑燊3,夏永军1,王光强1,胡 健3,艾连中1,*   

  1. 1.上海理工大学医疗器械与食品学院,上海 200093;2.江南大学 食品科学与技术国家重点实验室,江苏 无锡 214122;
    3.上海金枫酒业股份有限公司 上海黄酒工程技术研究中心,上海 20
  • 出版日期:2016-02-25 发布日期:2016-02-23
  • 通讯作者: 艾连中
  • 基金资助:

    上海市农业科技成果转化资金项目(133919N1000);上海市研究生创新基金项目(JWCXSL1402);
    沪江基金研究基地专项(D15012)

Development of an Analytical Method for Nine Biogenic Amines in Chinese Yellow Wine by HPLC

CAO Lirui1, ZHU Song2, YU Jianshen3, XIA Yongjun1, WANG Guangqiang1, HU Jian3, AI Lianzhong1,*   

  1. 1. School of Medical Instrument and Food Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China;
    2. State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214122, China;
    3. Shanghai Engineering Research Center of Chinese Rice Wine, Shanghai Jinfeng Wine Co. Ltd., Shanghai 201501, China
  • Online:2016-02-25 Published:2016-02-23
  • Contact: AI Lianzhong

摘要:

建立一种检测黄酒中生物胺的反相高效液相色谱法。用三氯乙酸提取黄酒中生物胺,丹磺酰氯作为衍生化试剂,1,7-二氨基庚烷作为内标定量。色谱条件为:Waters XBridge C18色谱柱(4.5 mm×250 mm,3.8 μm)作为分离柱,乙腈和水作为流动相进行梯度洗脱,流速1 mL/min,紫外检测波长254 nm。结果表明,9 种生物胺(盐酸吡哆胺、色胺、腐胺、尸胺、β-苯乙胺、组胺、酪胺、精胺和亚精胺)在40 min内能被很好分离。在1~50 mg/L质量浓度范围内,各种生物胺呈现良好的线性相关性(R2>0.999)。各生物胺加标回收率为79.54%~89.55%,相对标准偏差为3.14%~6.35%,该法各组分检出限(RSN=3)为0.002~0.009 mg/L。应用柱前衍生化高效液相色谱-紫外检测法,实现了黄酒中生物胺的准确检测。

关键词: 生物胺, 黄酒, 高效液相色谱法, 梯度洗脱

Abstract:

An analytical method for biogenic amines in Chinese rice wine by reversed phase high-performance liquid
chromatography (RP-HPLC-HPLC) was developed. The biogenic amines in Chinese yellow wine were extracted with
trichloroacetic acid (TCA), and then pre-column derivatized with dansyl chloride for quantification using 1,7-diamino
heptane as the quantitative internal standard. A C18 chromatographic column (4.5 mm × 250 mm, 3.8 μm) was used
for separation. The mobile phase was composed of a mixture of acetonitrile and water at a flow rate of 1 mL/min, and
the ultraviolet (UV) detection wavelength was 254 nm. The results showed that nine biogenic amines (pyridoxamine
dihydrochloride, tryptamine, putrescine, cadaverine, beta phenethylamine, histamine, tyramine, spermine and spermine)
were separated completely within 40 minutes. In the concentration range of 1–50 mg/L, each biogenic amine presented good
linear correlation (R2 > 0.999). After the addition of a mixed standard solution of biogenic amines to Chinese yellow wine,
the recovery rates were 79.54%–89.55%, with relative standard deviations (RSDs) ranging from 3.14% to 6.35%, and the
limit of detection for each component was 0.002–0.009 mg/L. Therefore, The HPLC method with pre-column derivatization
and UV detection could be used for the determination of biogenic amines in Chinese yellow wine.

Key words: biogenic amine, Chinese yellow wine, high performance liquid chromatography (HPLC), gradient elution

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