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郑凤家, 李蔚, 陈金东, 姜大峰, 李凤华, 王晓琳. 保健食品中低聚木糖高效液相色谱-示差折光法测定[J]. 中国公共卫生, 2020, 36(3): 429-432. DOI: 10.11847/zgggws1118570
引用本文: 郑凤家, 李蔚, 陈金东, 姜大峰, 李凤华, 王晓琳. 保健食品中低聚木糖高效液相色谱-示差折光法测定[J]. 中国公共卫生, 2020, 36(3): 429-432. DOI: 10.11847/zgggws1118570
Feng-jia ZHENG, Wei LI, Jin-dong CHEN, . Determination of xylo-oligosaccharides in health foods by high performance liquid chromatography with refractive index[J]. Chinese Journal of Public Health, 2020, 36(3): 429-432. DOI: 10.11847/zgggws1118570
Citation: Feng-jia ZHENG, Wei LI, Jin-dong CHEN, . Determination of xylo-oligosaccharides in health foods by high performance liquid chromatography with refractive index[J]. Chinese Journal of Public Health, 2020, 36(3): 429-432. DOI: 10.11847/zgggws1118570

保健食品中低聚木糖高效液相色谱-示差折光法测定

Determination of xylo-oligosaccharides in health foods by high performance liquid chromatography with refractive index

  • 摘要:
      目的  建立高效液相色谱硫酸水解法测定保健食品中低聚木糖(以木糖计)的方法。
      方法  样品经水提取30 min,低温下利用乙醇沉降大分子糖类,硫酸水解90 min,用氢氧化钠中和后,氨基柱分离,示差折光检测器检测,外标法定量,水解前后木糖含量之差即低聚木糖含量。
      结果  木糖浓度为0.25~5.00 mg/mL时,其质量浓度与峰面积线性关系良好(Y = 61 349.49X – 1 028.52,r = 0.999 9)。在保健食品中加标回收率为83.5 %~96.7 %,相对标准偏差(RSD)为1.67 %~4.82 %。低聚木糖检出限为1.1 g/kg,定量限为3.3 g/kg。
      结论  该方法准确、灵敏、方便、能够测定低聚木糖终端产品中的含量。

     

    Abstract:
      Objective  To develop a method for the determination of xylo-oligosaccharides (in xylose) in health foods by high performance liquid chromatography with refractive index (HPLC-RI).
      Methods  The samples were extracted with water for 30 minutes then higher molecular saccharides were precipitated with alcohol at low temperature. After subsequently hydrolyzed with sulfuric acid solution for 90 minutes, neutralized with sodium hydroxide solution and separated on a NH2 column, the samples were detected quantitatively with refractive index detector using external standard. The xylo-oligosaccharides content was measured based on the difference value for xylose concentration before and after the hydrolysis process.
      Results  A high linearity of the calibration curve between the peak area and the mass concentration of xylose was observed (Y = 61 349.49X – 1 028.52, r = 0.999 9) under the xylose concentration ranging between 0.25 – 5.00 mg/mL. The recovery rates were between 83.5% and 96.7% and the relative standard deviations ranged from 1.67% to 4.82% in health foods. The detection limit of the method is 1.1 g/kg and the quantification limit is 3.3 g/kg.
      Conclusion  The established method is accurate, sensitive, and simple and could be used for the determination of xylo-oligosaccharides in health foods.

     

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