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。
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.
作者
张冰冰
欧则民
严林
张瑶
王艳静
程怡
仝燕
梁爱华
刘德文
王锦玉
ZHANG Bing-bing;OU Ze-min;YAN Lin;ZHANG Yao;WANG Yan-jing;CHENG Yi;TONG Yan;LIANG Ai-hua;LIU De-wen;WANG Jin-yu(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;School of Pharmacy,Jiangxi University of Chinese Medicine,Nanchang 330004,China;School of Pharmacy,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2022年第11期156-163,共8页
Chinese Journal of Experimental Traditional Medical Formulae
基金
中国中医科学院基金项目(CI2021A04801,ZZ-13-035-10)
中国中医科学院中药研究所团队建设基金项目(ZXKT19014)。
关键词
栀子
大孔树脂
环烯醚萜
西红花苷
正交试验
超高效液相色谱法(UPLC)
纯化工艺
Gardeniae Fructus
macroporous resin
iridoid
crocin
orthogonal test
ultra-high performance liquid chromatography(UPLC)
purification process
