CN104311624B - A kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly - Google Patents
A kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly Download PDFInfo
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- CN104311624B CN104311624B CN201410522145.8A CN201410522145A CN104311624B CN 104311624 B CN104311624 B CN 104311624B CN 201410522145 A CN201410522145 A CN 201410522145A CN 104311624 B CN104311624 B CN 104311624B
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- chinese holly
- saponin
- holly
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Steroid Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly, comprise the steps: Feedstock treating, the process of high pressure microjet micronizing, high pressure extract, collect the extracting solution obtained after having extracted, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, use the ethanolic soln wash-out of 50-60% again, through concentrated, spraying dry, obtain Leaf of Chinese Holly saponin.Have content high, extraction yield is high, and technique is simple, is applicable to producing, the advantages such as production cost is low.
Description
Technical field
The present invention relates to the extracting method of biological technical field, is a kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly specifically.
Background technology
Leaf of Chinese Holly (IlexkudingchaC.J.Tseng), English name: LeafofChineseHolly, leafofBroadleafHolly, it is Aquifoliaceae Ilex latifolia Thunb kind aiphyllium, be commonly called as tea fourth, Fu Dingcha, highland Lu's tea, mainly being distributed in the ground such as southwest (Sichuan, Chongqing, Guizhou, Hunan, Hubei) and South China (Jiangxi, Yunnan, Guangdong, Fujian, Hainan), is a kind of traditional pure natural health-care beverage good merchantable brand of China.Containing 200 Multiple components such as bitter leaves saponin, amino acid, vitamins C, Polyphenols, flavonoid, trimethyl-xanthine, protein in Leaf of Chinese Holly.Its delicate fragrance that becomes to sample tea has bitter taste, then sweet cool, there is clearing away heat and removing summer, eyesight-improving intelligence-developing, promote the production of body fluid to quench thirst, diuresis cardiac stimulant, the cough-relieving that wets one's whistle, step-down fat-reducing, press down cancer anti-cancer, anti-ageing, the multiple efficacies such as arteries and veins of invigorating blood circulation, have the laudatory title such as " health tea ", " cosmetic tea ", " diet tea ", " blood-pressure decreasing tea ", " lengthen one's life tea ".The plurality kinds of health care food such as bag bubble Leaf of Chinese Holly, Leaf of Chinese Holly electuary, buccal lozenge of lectuce tea, compound Leaf of Chinese Holly.
But certain alkaloid component in Leaf of Chinese Holly has bitter cold characteristic, be not therefore that everybody is suitable for drinking Leaf of Chinese Holly, suffered from the people of common cold caused by wind-cold, the people of cold of insufficiency type physique, chronic gastroenteritis patient can not drink, menstruating women and new puerpera are also not suitable for drinking.And Leaf of Chinese Holly complicated component, its active constituent content is limited, comparatively large as usage quantity during drug use, but Leaf of Chinese Holly bitter taste is dense, and mouthfeel is bad, should not be accepted.In order to remove bitter cold material in Leaf of Chinese Holly, retain its activeconstituents, need to carry out purification processes in Leaf of Chinese Holly, the extraction as active components of plants adopts the methods such as solvent extration, macroreticular resin absorbing method, solvent precipitation, solvent precipitation, the cholesterol precipitator method, lead salt precipitation, chromatography more.But these methods exist some defects, such as: solvent extration length consuming time, easily occurs emulsion layer, have a strong impact on effect of extracting and the purity of general glycoside, this method should not to the process of a large amount of sample; Macroreticular resin absorbing method: the grease in plant, lipotropic component or low polarity component are easy to be combined with macroporous resin, last layer oil layer is coated with at resin surface, and the solvent elution of macroporous resin be water or hydrophilic solvent time, greatly will reduce the absorption carrying capacity of macroporous resin, have a strong impact on separating effect; Solvent precipitation needs the organic solvent adding high times amount, and consumption of organic solvent is large, has pollution to environment, and concentrated comparatively difficulty, extract purity is also low, also there is organic problem of solvent residual; The cholesterol precipitator method: the molecular complex less stable that cornutaside and sterol are formed, are not suitable for purifying by the cholesterol precipitator method; Lead salt precipitation: technique is more complicated, deleading technique is difficult, and content of heavy metal lead is high, and product colour is very dark, is difficult to reach food and drug standard requirement; Chromatography: this method and resin method technique similar, also have the defect the same with macroreticular resin absorbing method, in addition the too large inferior separating effect of the granularity of chromatography aluminum oxide, the too little solvent flow rate of granularity is slow, easily makes diffusion of bands.
Summary of the invention
The object of this invention is to provide a kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly, there is technique simple, be applicable to producing, the advantages such as production cost is low, by Leaf of Chinese Holly saponin content in the product of the method extraction gained more than 95%, extraction yield more than 85%.
The present invention is achieved through the following technical solutions, and specifically comprises the steps:
1) Feedstock treating: the blade of Leaf of Chinese Holly is pulverized;
2) high pressure microjet micronizing process: the Leaf of Chinese Holly after pulverizing is added pure water according to the weight ratio of 1:8-10, with high-speed shearing emulsion machine process 10-20min, rotating speed is 8000-12000r/min, then process in 25 DEG C with high pressure microjet Ultra-Micro Grinding Equipment, processing pressure is 80-120MPa, number of processes is 2-4 time, obtains paste serous material;
3) high pressure extract: by step 1) paste serous material that obtains, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10-15min, recover normal pressure, obtain extracting solution;
4) extracting solution obtained after collecting high pressure extract, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, then uses the ethanolic soln wash-out of 50-60%, through concentrated, spraying dry, obtains Leaf of Chinese Holly saponin.
Step 1 of the present invention) described in Leaf of Chinese Holly be that holly plant Chinese holly is or/and Cortex Ilicis Rotundae is or/and the leaf of Kudincha Holly.
Step 4) described in AB-8 resin column, resin demand be the 40-60 of supernatant liquor weight doubly.
The Leaf of Chinese Holly saponin that the present invention obtains, detect through HPLC, content is more than 95%.
Compared with prior art, advantage of the present invention:
1, prior art is when carrying out the extraction of the compositions such as Leaf of Chinese Holly saponin, pre-treatment is all generally for solvent with water or ethanol etc., by heating extraction by effective constituent stripping, and the present invention adopts high pressure microjet micronizing to process Leaf of Chinese Holly raw material, in conjunction with high pressure extract, compare heating to extract, through the effect of high pressure micronizing, make the trimethyl-xanthine contained in Leaf of Chinese Holly, saponin, tannin, the composition energy fully strippings such as amaroid, be beneficial to the process of subsequent technique, be beneficial to the yield improving activeconstituents, and, avoid the destruction of high temperature to Leaf of Chinese Holly effective constituent.
2, the Leaf of Chinese Holly saponin content that prior art obtains generally is no more than 95%, the present invention adopts the combination of high pressure microjet superfine communication technique, high pressure extract and Adsorption technology, along with adding of high pressure microjet superfine communication technique, combine with technique of the present invention is made to occur the raising of matter, compare column chromatography after water extraction or alcohol extracting, time of the present invention is short, and Leaf of Chinese Holly saponin content is high; Compare supercritical CO
2fluid extraction adds column chromatography, extraction yield more than 85% of the present invention.
3, present invention, avoiding the use of a large amount of organic solvent such as dehydrated alcohol, methyl alcohol, environmental protection more.
Embodiment
With embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1:
From Leaf of Chinese Holly, extract a method for Leaf of Chinese Holly saponin, specifically comprise the steps:
1) Feedstock treating: the blade 100kg of Cortex Ilicis Rotundae is pulverized;
2) high pressure microjet micronizing process: the Leaf of Chinese Holly after pulverizing is added 800kg pure water, with high-speed shearing emulsion machine process 10min, rotating speed is 12000r/min, then process in 25 DEG C with high pressure microjet Ultra-Micro Grinding Equipment, processing pressure is 100MPa, number of processes is 3 times, obtains paste serous material;
3) high pressure extract: by step 1) paste serous material that obtains, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10min, recover normal pressure, obtain extracting solution;
4) extracting solution obtained after collecting high pressure extract, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, then uses the ethanolic soln wash-out of 50-60%, through concentrated, spraying dry, obtains Leaf of Chinese Holly saponin.
Embodiment 2:
From Leaf of Chinese Holly, extract a method for Leaf of Chinese Holly saponin, specifically comprise the steps:
1) Feedstock treating: the blade 100kg of Kudincha Holly is pulverized;
2) high pressure microjet micronizing process: the Leaf of Chinese Holly after pulverizing is added pure water 1000kg, with high-speed shearing emulsion machine process 15min, rotating speed is 10000r/min, then process in 25 DEG C with high pressure microjet Ultra-Micro Grinding Equipment, processing pressure is 80MPa, number of processes is 4 times, obtains paste serous material;
3) high pressure extract: by step 1) paste serous material that obtains, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 12min, recover normal pressure, obtain extracting solution;
4) extracting solution obtained after collecting high pressure extract, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, then uses the ethanolic soln wash-out of 50-60%, through concentrated, spraying dry, obtains Leaf of Chinese Holly saponin.
Embodiment 3:
1) Feedstock treating: the blade 100kg of Chinese holly and Cortex Ilicis Rotundae is pulverized;
2) high pressure microjet micronizing process: the Leaf of Chinese Holly after pulverizing is added pure water 900kg, with high-speed shearing emulsion machine process 20min, rotating speed is 8000r/min, then process in 25 DEG C with high pressure microjet Ultra-Micro Grinding Equipment, processing pressure is 120MPa, number of processes is 2 times, obtains paste serous material;
3) high pressure extract: by step 1) paste serous material that obtains, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 15min, recover normal pressure, obtain extracting solution;
4) extracting solution obtained after collecting high pressure extract, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, then uses the ethanolic soln wash-out of 50-60%, through concentrated, spraying dry, obtains Leaf of Chinese Holly saponin.
Result:
Claims (3)
1. from Leaf of Chinese Holly, extract a method for Leaf of Chinese Holly saponin, it is characterized in that:
Specifically comprise the steps:
1) Feedstock treating: the blade of Leaf of Chinese Holly is pulverized;
2) high pressure microjet micronizing process: the Leaf of Chinese Holly after pulverizing is added pure water according to the weight ratio of 1:8-10, with high-speed shearing emulsion machine process 10-20min, rotating speed is 8000-12000r/min, then process in 25 DEG C with high pressure microjet Ultra-Micro Grinding Equipment, processing pressure is 80-120MPa, number of processes is 2-4 time, obtains paste serous material;
3) high pressure extract: by step 2) paste serous material that obtains, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10-15min, recover normal pressure, obtain extracting solution;
4) extracting solution obtained after collecting high pressure extract, centrifugal, supernatant liquor carries out AB-8 resin column chromatography, then uses the ethanolic soln wash-out of 50-60%, through concentrated, spraying dry, obtains Leaf of Chinese Holly saponin.
2. a kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly according to claim 1, is characterized in that: step 1) described in Leaf of Chinese Holly be that holly plant Chinese holly is or/and Cortex Ilicis Rotundae is or/and the leaf of Kudincha Holly.
3. a kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly according to claim 1, is characterized in that: step 4) described in AB-8 resin column, resin demand be the 40-60 of supernatant liquor weight doubly.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410522145.8A CN104311624B (en) | 2014-09-30 | 2014-09-30 | A kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly |
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| CN201410522145.8A CN104311624B (en) | 2014-09-30 | 2014-09-30 | A kind of method extracting Leaf of Chinese Holly saponin from Leaf of Chinese Holly |
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| CN104311624A CN104311624A (en) | 2015-01-28 |
| CN104311624B true CN104311624B (en) | 2016-04-27 |
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| CN105052542A (en) * | 2015-07-31 | 2015-11-18 | 桂林宏旺菌业股份有限公司 | Black fungus cultivation method |
| CN108077480A (en) * | 2018-01-15 | 2018-05-29 | 浦北县利民农产品产销专业合作社 | It can persistently keep brewing golden flower fruit teas of color and luster and preparation method thereof |
| CN107950720A (en) * | 2018-01-15 | 2018-04-24 | 浦北县利民农产品产销专业合作社 | It can persistently keep brewing yearning between lovers fruit tea of color and luster and preparation method thereof |
| CN115919910A (en) * | 2022-08-25 | 2023-04-07 | 琛蓝(美国)营养制品股份有限公司 | Bitter-removed broadleaf holly leaf extract with anti-fatigue effect, preparation method and fingerprint detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1202121C (en) * | 2002-12-18 | 2005-05-18 | 中南大学 | Method for extracting total triterpenic acid, ursolic acid and oleanolic acid from Taiwan lectuce herb tea |
| CN101016328B (en) * | 2007-02-09 | 2010-09-29 | 江苏久吾高科技股份有限公司 | Method of separating and purifying ursolic acid and oleanolic acid |
| CN101284031B (en) * | 2008-06-03 | 2011-05-04 | 上海雷允上科技发展有限公司 | Hairy holly root extract, its preparation and application |
| CN101775061A (en) * | 2009-09-15 | 2010-07-14 | 沈阳药科大学 | Ilex latifolia thunb saponin compound |
| CN102649806A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Preparation method of pedunculoside |
| CN102329365A (en) * | 2011-07-06 | 2012-01-25 | 南京泽朗农业发展有限公司 | Method for separating and preparing ilexin II |
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