色谱 ›› 2015, Vol. 33 ›› Issue (6): 662-666.DOI: 10.3724/SP.J.1123.2015.02053

• 技术与应用 • 上一篇    下一篇

高效阴离子交换色谱-积分脉冲安培检测法同时测定黄酒中的单糖和低聚糖及其指纹图谱的构建

胡贝贞1, 董文洪1, 夏碧琪2, 宋伟华1, 韩超2   

  1. 1. 绍兴出入境检验检疫局, 浙江 绍兴 312000;
    2. 温州出入境检验检疫局, 浙江 温州 325027
  • 收稿日期:2015-02-05 发布日期:2015-05-26
  • 通讯作者: 韩超
  • 基金资助:

    浙江出入境检验检疫局科技计划项目(ZK201321).

Simultaneous determination of monosaccharide and oligosaccharide in rice wine by high performance anion exchange chromatography with integrated pulsed amperometric detection and the establishment of their fingerprints

HU Beizhen1, DONG Wenhong1, XIA Biqi2, SONG Weihua1, HAN Chao2   

  1. 1. Shaoxing Entry-Exit Inspection and Quarantine Bureau, Shaoxing 312000, China;
    2. Wenzhou Entry-Exit Inspection and Quarantine Bureau, Wenzhou 325027, China
  • Received:2015-02-05 Published:2015-05-26

摘要:

建立了黄酒中葡萄糖、果糖、异麦芽糖、异麦芽三糖、麦芽糖、潘糖、麦芽三糖共7种糖类的高效阴离子交换色谱分离-积分脉冲安培检测的方法。以氢氧化钠和醋酸钠为淋洗液进行梯度洗脱,CarboPacTM10阴离子交换柱进行分离。该方法可在26 min内实现黄酒中7种糖类的定量分析,在0.5~50 mg/L浓度范围内线性关系良好,样品定量限为0.1 g/L,加标回收率为76.5%~108.4%,精密度(RSD)为3.02%~8.23%。将该法用于不同厂家不同批次的绍兴加饭酒中各种糖类含量的检测,基于所得的检测结果,利用中位数法构建了标准指纹图谱,并采用夹角余弦法评价了各个样品与标准指纹图谱之间的相似度。结果初步显示,不同厂家加饭酒之间的相似度差别较大,该法可作为区别不同厂家酒的依据之一。

关键词: 单糖, 低聚糖, 高效阴离子交换色谱, 黄酒, 积分脉冲安培检测, 指纹图谱

Abstract:

An analytical method for the determination of glucose, fructose, isomaltose, isomaltotriose, maltose, panose and maltotriose was developed by high performance anion exchange chromatography coupled with integrated pulsed amperometric detection. The analysis was performed on a CarboPacTM10 column with gradient elution of NaOH-NaOAc as mobile phases. The seven sugars were well separated in less than 26 min and showed good linear correlation coefficients between 0.5 and 50 mg/L. The detection limits (LODs) were 0.1 g/L. The recoveries ranged from 76.5% to 108.4% at different spiked levels. The relative standard deviations were between 3.02% and 8.23%. The established method was applied in determining the seven sugars in different batches of Shaoxing Jiafan rice wines from different manufacturers. The standard fingerprints were established by median values using the obtained results. Similarities of the fingerprints of the samples to the standard were calculated by using angle cosine. The results showed that the similarities of wines from different manufacturers were significantly different, so the method could be used for the identification of rice wines from different manufacturers.

Key words: fingerprints, high performance anion exchange chromatography (HPAEC), integrated pulsed amperometric detection (PAD), monosaccharide, oligosaccharide, rice wines

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