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诃黎勒酸和诃子酸的提取、分离工艺优化
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| 篇名： | 诃黎勒酸和诃子酸的提取、分离工艺优化 |
| TITLE： | Optimization of the extraction and separation process of chebulagic acid and chebulinic acid |
| 摘要： | 目的优化诃子中诃黎勒酸和诃子酸的提取、分离工艺。方法在单因素实验基础上，以物料粒径、液料比、提取时间、提取次数为考察因素，以诃黎勒酸、诃子酸含量为指标，采用正交实验设计优化诃黎勒酸和诃子酸的提取工艺。以上样液浓度、洗脱溶剂、十八烷基键合硅胶反相填料（ODS）用量与上样生药量比值为考察因素，优化诃黎勒酸和诃子酸的分离工艺。结果诃黎勒酸和诃子酸的最佳提取工艺为乙醇体积分数70%，超声提取，物料粒径120目，液料比25∶1（mL/g），提取时间20min，提取次数2次；经3次实验验证，平均综合得分为99.33分（RSD＝0.68%，n＝3），诃黎勒酸、诃子酸的平均含量分别为107.05、58.32mg/g。诃黎勒酸和诃子酸的最佳分离工艺为上样液浓度0.5g/mL（1mL相当于0.5g药材），ODS用量与上样生药量比值10∶1.5（g/g），甲醇-水（1∶4，V/V）洗脱诃黎勒酸，甲醇-水（3∶7，V/V）洗脱诃子酸；经3次实验验证，诃黎勒酸、诃子酸的平均总得率分别为53.33%、39.23%。经重结晶后，2种成分的纯度均为100%。结论所建立的诃黎勒酸和诃子酸的提取、分离工艺简单可行。 |
| ABSTRACT： | OBJECTIVE To optimize the extraction and separation process of chebulagic acid and chebulinic acid from Terminalia chebula. METHODS Based on single factor experiment， with particle size， liquid-solid ratio， extraction time and extraction times as factors， using the contents of chebulagic acid and chebulinic acid as indexes， orthogonal experiment was designed to optimize the extraction process of chebulagic acid and chebulinic acid. Taking sample concentration， elution solvent and the ratio of eighteen-group bonded silicone reverse phase （ODS） to the amount of raw medicine as factors， the separation processes of chebulagic acid and chebulinic acid were optimized. RESULTS The optimal extraction process of chebulagic acid and chebulinic acid included ethanol volume fraction of 70%， ultrasonic extraction， particle size of 120 mesh， liquid-solid ratio of 25∶1 （mL/g）， extraction time of 20 min， and extracting for 2 times. After 3 experiments， the average comprehensive score was 99.33 （RSD＝ 0.68%， n＝3）， and the average contents of chebulagic acid and chebulinic acid were 107.05 and 58.32 mg/g， respectively. The optimal separation process of the two components included the concentration of sample loading solution was 0.5 g/mL （1 mL was equivalent to 0.5 g of medicinal materials）， the ratio of ODS to the amount of raw medicine was 10∶1.5 （g/g）， methanol-water （1∶4， V/V） eluted chebulagic acid， methanol-water （3∶7， V/V） eluted chebulinic acid. After 3 experiments， the average total yields of the two components were 53.33%， 39.23%. After recrystallization， the purity of both components was 100%. CONCLUSIONS Established extraction and separation process of chebulagic acid and chebulinic acid is simple and feasible. |
| 期刊： | 2022年第33卷第22期 |
| 作者： | 陈九妹，朱麒臻，鞠成国，张强，王巍 |
| AUTHORS： | CHEN Jiumei，ZHU Qizhen，JU Chengguo，ZHANG Qiang，WANG Wei |
| 关键字： | 诃黎勒酸；诃子酸；提取工艺；分离工艺 |
| KEYWORDS： | chebulagic acid； chebulinic acid； extraction process； separation process |
| 阅读数： | 169 次 |
| 本月下载数： | 2 次 |
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