摘要
建立了一种灵敏、特异、精确定量分析花椒叶多糖的苯酚-硫酸法,采用该方法测定了陕西大红袍花椒叶中多糖的含量。该方法选择半乳糖作为标准单糖,484nm为工作波长。通过单因素实验和正交试验优化得到了较佳显色反应条件是加样次序为苯酚-样品-浓硫酸,显色温度为25℃,质量分数为5%的苯酚添加量为0.3mL,浓硫酸添加量为3.5mL,显色时间为30min。系统适应性实验显示该方法的标准曲线方程为y=0.0127x-0.0076(R^2=0.997),线性范围为10.00—60.00μg/mL,LOD和LOQ分别为2.08μg/mL和6.30μg/mL,日内、日间精密度分别在0.49%~3.64%,5.17%~6.05%之间,平均回收率为101.19%。样品溶液在显色反应后的2h内稳定性较好。测定发现陕西大红袍花椒叶中ω(多糖)在8.11~8.89mg/g之间。该方法为花椒叶多糖的定量分析和花椒叶资源的开发利用提供了参考。
A sensitive, specific, accurate and precise phenol-sulfuric acid method was established for quantitative assay of polysaccharides in Zanthoxylum bungeanum leaves. And polysaccharides in leaves of Dahongpao, a cultivar of Z. bungeanum in Shaanxi province, were successfully determinated by the proposed phenol-sulfuric acid method. Galactose was used as standard monosaccharide and 484nm was cho- sen as working wavelength. The optimum conditions for chromogenic reaction were obtained by single factor experiments and orthogonal test: addition sequence, phenol-sample-concentrated sulfuric acid; temperature of chromogenic reaction, 25 ℃ ; amount of 5% phenol, 0.3 mL; amount of concentrated sulfuric acid, 3.5 mL; and duration of chromogenic reaction, 30 min. System suitability test indicated that regression equation of standard curve was y =0. 012 7x -0. 007 6 (R^2 =0. 997) and range with satisfactory accuracy and precision was 10.00 - 60.00 μg/mL. LOD and LOQ were 2.08 μg/mL and 6.30 μg/mL, respectively. Intra-and inter-day precision varied from 0.49% to 3.64% and from 5.17% to 6.05% , respectively. And mean recovery was 101.19%. The colored sample solution was stable within 2 h. The content of polysaccharides in Dahongpao leaves in Shaanxi province, was in the range of 8. 11 -8. 89 mg/g. The developed colorimetric method provides a basis for quantification of polysaccharides from Z. bungeanum leaves and exploitation of leaf resources.
出处
《食品科学技术学报》
CAS
2015年第4期40-46,共7页
Journal of Food Science and Technology
基金
中央高校基本科研业务费专项资金项目(GK201302048)
陕西省大学生创新创业训练计划项目(cx13063)
关键词
花椒叶
多糖
苯酚-硫酸法
显色反应
Zanthoxylum bungeanum leaves
polysaccharides
phenol-sulfuric acid method
chromogenic reaction