食品科学

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长白落叶松中花旗松素的结构鉴定与含量测定

张卫鹏,刘 伟,付警辉,柴 婧,刘文丛,郑毅男   

  1. 1.吉林农业大学中药材学院,吉林 长春 130118;2.吉林省轻工业设计研究院, 吉林 长春 130021;
    3.吉林农业大学资源与环境学院,吉林 长春 130118
  • 出版日期:2013-08-25 发布日期:2013-09-03

Structural Identification and Quantitative Analysis of Taxifolin in Larix olgensis Henry var. koreana Nakai

ZHANG Wei-peng,LIU Wei,FU Jing-hui,CHAI Jing,LIU Wen-cong,ZHENG Yi-nan   

  1. 1. College of Chinese Medicinal Materials, Jilin Agricultural University, Changchun 130118, China;
    2. Jilin Provincial Light Industry Design and Research Institute, Changchun 130021, China;
    3. College of Resources and Environment, Jilin Agricultural University, Changchun 130118, China
  • Online:2013-08-25 Published:2013-09-03

摘要:

目的:从长白落叶松中分离花旗松素并对其进行结构鉴定;采用高效液相色谱法测定临江地区长白落叶松根上部横切面及11个林场长白落叶松中花旗松素的含量。方法:色谱柱:15C18-AR Waters(6mm×250mm,5μm);检测波长:288nm;流动相:甲醇-水(40:60,V/V);流速:1mL/min;柱温:30℃;进样量:20μL。结果:与研究报道比较,紫外、红外、质谱和核磁共振碳谱所得数据一致,证明所得提取物为花旗松素;在0.05~1.0mg/mL范围内质量浓度与峰面积呈现良好线性关系,r=0.9998,平均回收率为99.3%,相对标准偏差(RSD)为2.6%(n=9);长白落叶松中花旗松素含量沿横切面由内至外呈递减分布,同时受生长条件影响较大。结论:本法操作简便、准确、专属性强、重复性好,可用作长白落叶松中花旗松素的含量测定。

关键词: 长白落叶松, 花旗松素, 结构鉴定, 高效液相色谱法, 含量测定

Abstract:

Objective: To identify structurally the taxifolin from Larix olgensis Henry var. koreana Nakai and determinate
taxifolin content in the cross section of upper roots of Larix olgensis Henry var. koreana Nakai from Lijiang region of Jilin
province and in trees from 11 forest farms. Methods: Chromatographic separation was performed on a 15C18-AR waters column
(6 mm × 250 mm, 5 μm) with methanol/water (40:60, V/V) as the mobile phase at a flow rate of 1 mL/min. The column
temperature was 30 ℃. UV detection was performed at 288 nm. The injection volume was 20 μL. Results: The IR, UV, MS and
13C-NMR data obtained were consistent with those reported in the literature confirming the extract to be taxifolin. A good linear
relationship between peak area and taxifolin concentration in the range of 0.05 to 1.0 mg/mL was observed with correlation
coefficient r = 0. 9998. The average recovery of taxifolin was 99.3% with RSD of 2.6% (n = 9). In upper roots of Larix olgensis
Henry var. koreana Nakai, taxifolin was distributed in a gradually decreasing amount from pith to bark and also affected greatly
by growth conditions. Conclusion: The analytical method presented in this study proved simple, acurate, specific, repeatable
and applicable for quantitative analysis of taxifolin from Larix olgensis Henry var. koreana Nakai.

Key words: Larix olgensis Henry var. koreana Nakai, taxifolin, structural identification, high performance liquid chromatography (HPLC), content determination