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草果总黄酮的大孔吸附树脂纯化工艺优化研究
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| 篇名： | 草果总黄酮的大孔吸附树脂纯化工艺优化研究 |
| TITLE： | Study on the Optimization of Purification Technology of Total Flavonoids from Amomum tsao-ko by Macroporous Adsorption Resin |
| 摘要： | 目的：建立草果总黄酮的含量测定方法，并对其大孔吸附树脂纯化工艺进行优化。方法：采用高效液相色谱法测定草果中总黄酮的含量。色谱柱为EclipsePlusC18，流动相为乙腈-1％醋酸水溶液（15∶85，V/V），柱温为40℃，流速为0.8mL/min，检测波长为256nm，进样量为10μL。以吸附、解吸性能为考察指标，采用静态吸附和解吸试验对6种大孔吸附树脂进行筛选，采用静态吸附和解吸动力学试验考察吸附和解吸时间。在单因素试验的基础上，以总黄酮含量（以芦丁计）为评价指标，以上样液质量浓度、上样液pH、乙醇体积分数及洗脱用量为考察因素，采用正交设计优化草果总黄酮的纯化工艺并进行验证试验。结果：芦丁检测质量浓度的线性范围为0.028～0.281mg/mL（r＝0.9999）；定量限为437.5ng/mL，检测限为109.4ng/mL；精密度、稳定性、重复性试验的RSD均小于2％，加样回收率为96.24％～99.75％（RSD＜2％，n＝6）。HPD450型大孔吸附树脂对草果总黄酮的静态吸附和解吸综合能力最适中，最佳静态吸附与解吸时间均为12h。最优纯化工艺为上样质量浓度1.8544mg/mL，上样液pH7，乙醇体积分数60％，乙醇洗脱用量8倍柱体积。验证试验显示，按最优工艺纯化后的草果总黄酮含量由纯化前的22.5567mg/g上升至57.7282mg/g，纯化倍数为2.56（n＝3）。结论：所建含量测定方法灵敏度高、稳定性好，优化的纯化工艺稳定、可行，可用于草果总黄酮的纯化。 |
| ABSTRACT： | OBJECTIVE：To establish a method for the content determination of to tal flavonoids from Amomum tsao-ko ，and to optimize the purification technology by macroporous resin. METHODS ：The content of total flavonoids was measured by HPLC. The determination was performed on Eclipse Plus C 18 column with mobile phase consisted of acetonitrile- 1％ acetic acid solution （15∶85，V/V）at the flow rate of 0.8 mL/min. The column temperature was 40 ℃，and the detection wavelength was set at 256 nm. The sample size was 10 μL. Taking the adsorption and desorption performance as indexes，6 kinds of macroporous resins were screened out by static adsorption and desorption tests ；adsorption and desorption time were investigated by static adsorption and desorption kinetics tests. Using the content of total flavonoids （calculated by rutin ）as index ，with sample concentration ，sample pH，ethanol volume fraction and elution amount as factors ，based on single factor test ，orthogonal design was used to optimize the purification technology of total flavonoids from A. tsao-ko ，and validation test was performed. RESULTS ：The linear range of rutin were 0.028-0.281 mg/mL（r＝0.999 9）. The limit of quantification was 437.5 ng/mL and the limit of detection was 109.4 ng/mL. RSDs of precision ，stability and reproducibility tests were all lower than 2％；the recoveries were 96.24％-99.75％（RSD＜2％，n＝ 6）. The comprehensive capacity of adsorption and desorption of HPD 450 macroporous resin was the most suitable ，and the best static adsorption and desorption time both were 12 h. The optimal purification technology was 1.854 4 mg/mL ； ethanol elution was 8 times of the column volume. Vertificationtests show that after optimized ，the content of total flavonoids from A. tsao-ko increased from 22.556 7 mg/g to 57.728 2 mg/g. The purity of was 2.56 and stable for the content determination. Optimal purification technology is stable and feasible ，which is suitable for purifieation of total flavonoids from A. tsao-ko . |
| 期刊： | 2020年第31卷第07期 |
| 作者： | 赵雨鸿，沈华，代双亿，蒲忠慧，谢子锐，肖灵，况敏，代敏 |
| AUTHORS： | ZHAO Yuhong ，SHEN Hua，DAI Shuangyi ，PU Zhonghui ，XIE Zirui，XIAO Ling，KUANG Min，DAI Min |
| 关键字： | 草果；总黄酮；含量测定；大孔吸附树脂；纯化工艺 |
| KEYWORDS： | Amomum tsao-ko ；Total flavonoids ；Content determination ；Macroporous absorption resin ；Purification technology |
| 阅读数： | 284 次 |
| 本月下载数： | 7 次 |
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