Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus

Bing-bing ZHANG; Ze-min OU; Lin YAN; Yao ZHANG; Yan-jing WANG; Yi CHENG; Yan TONG; Ai-hua LIANG; De-wen LIU; Jin-yu WANG

doi:10.13422/j.cnki.syfjx.20220153

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Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus

更新时间：2022-04-28

- Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 28, Issue 11, Pages: 156-163(2022)
- 作者机构：
  
  1.中国中医科学院中药研究所，北京 100700
  2.江西中医药大学药学院，南昌 330004
  3.天津中医药大学药学院，天津 301617
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20220153
  CLC： R22;R28;R943;R914
- Received：25 October 2021，
  
  Published Online：28 December 2021，
  
  Published：05 June 2022
- 稿件说明：
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张冰冰,欧则民,严林等.栀子总环烯醚萜和总西红花苷的提取纯化工艺考察[J].中国实验方剂学杂志,2022,28(11):156-163.

ZHANG Bing-bing,OU Ze-min,YAN Lin,et al.Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(11):156-163.
张冰冰,欧则民,严林等.栀子总环烯醚萜和总西红花苷的提取纯化工艺考察[J].中国实验方剂学杂志,2022,28(11):156-163. DOI： 10.13422/j.cnki.syfjx.20220153.

ZHANG Bing-bing,OU Ze-min,YAN Lin,et al.Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(11):156-163. DOI： 10.13422/j.cnki.syfjx.20220153.

摘要

目的

优化可用于工业化生产的栀子提取纯化工艺，得到总环烯醚萜和总西红花苷提取物。

方法

采用正交试验，以京尼平苷、京尼平龙胆双糖苷、羟异栀子苷、西红花苷-1和西红花苷-2含量为评价指标，考察煎煮时间、煎煮次数和加水量，优选栀子水提取工艺；采用单因素试验优选栀子水提物的纯化工艺，筛选4种不同类型的大孔吸附树脂，主要考察树脂型号、最大上样量、水洗用量、乙醇体积分数、洗脱剂用量、上样流速等工艺条件；此外，对提取物的干燥方式（真空干燥和喷雾干燥）进行考察，并进行中试放大验证试验。

结果

栀子的最佳水提取工艺为分别加15、10倍量水煎煮2次，每次1 h；最佳纯化工艺为水提取液滤过后通过SP825L型大孔树脂柱，生药量-树脂量（1∶1.5），药液上样流速3 BV·h

-1

，加水2 BV除杂，加30%乙醇4 BV洗脱得环烯醚萜部位，继续加70%乙醇3 BV洗脱得西红花苷部位，收集醇洗液，70 ℃减压干燥。在该条件下，总环烯醚萜提取量590.75 mg·g

-1

，转移率70.48%，干膏得率8.89%；总西红花苷提取量83.37 mg·g

-1

，转移率22.20%，干膏得率2.60%。

结论

优选的提取纯化工艺稳定可行，有效成分提取率高，适合栀子有效部位的工业化提取纯化。

Abstract

Objective

To optimize the extraction and purification process of Gardeniae Fructus for industrial production， and to obtain the total iridoid and total crocin extracts.

Method

Orthogonal test was used to optimize the water extraction process by taking contents of geniposide， genipin gentiobioside， gardenoside， crocin-1 and crocin-2 as indicators and the decocting time， decocting times and water amount as factors. The purification process was optimized by single factor test， and four different types of macroporous adsorption resins were screened. The process conditions such as resin type， maximum loading amount， water washing amount， ethanol concentration， ethanol dosage， and flow rate of sample loading were mainly investigated. In addition， the drying methods （vacuum drying and spray drying） of the extract were investigated， and a pilot scale-up verification test was carried out.

Result

The optimal water extraction process of Gardeniae Fructus was to add 15， 10 times the amount of water for decocting twice， 1 h each time. The optimal purification process was as follows：the water extract through SP825L macroporous resin column， the amount of crude drug-the amount of resin （1∶1.5）， the sample loading flow rate of 3 BV h

-1

， adding 2 BV of water to remove impurities， adding 4 BV of 30% ethanol to obtain the iridoid part， then adding 3 BV of 70% ethanol to obtain the crocin part， collecting the ethanol lotion， and drying at 70 ℃. Under these conditions， the extraction amount of total iridoids was 590.75 mg·g

-1

with the transfer rate of 70.48%， and the yield of dry extract was 8.89%. The extraction amount of total crocins was 83.37 mg·g

-1

with the transfer rate of 22.20%， and the dry extract yield was 2.60%.

Conclusion

The optimized extraction and purification process is stable and feasible with high extraction rate of active components， which is suitable for the industrial extraction and purification of active parts of Gardeniae Fructus.

关键词

Keywords

references

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