CN107903293A - A kind of extraction process of Camellia nitidissima saponin extract - Google Patents
A kind of extraction process of Camellia nitidissima saponin extract Download PDFInfo
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- CN107903293A CN107903293A CN201711189264.6A CN201711189264A CN107903293A CN 107903293 A CN107903293 A CN 107903293A CN 201711189264 A CN201711189264 A CN 201711189264A CN 107903293 A CN107903293 A CN 107903293A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
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Abstract
The invention discloses a kind of extraction process of Camellia nitidissima saponin extract, include the following steps：(1) golden camellia tea fragment is added to the water, and extracts 2 5h in 50 80 DEG C, then isolated Aqueous extracts and impurity；Impurity is added to the water, 2 5h is extracted again in 50 80 DEG C, separates again, Aqueous extracts are made；Then Aqueous extracts twice are eluted with solvent by macroporous absorbent resin, collects eluent；(2) precipitating reagent of its volume 1/5 1/10 is added into eluent, reacts 30 60min in 40 60 DEG C, then the precipitation containing tea saponin of isolated lower floor's generation；(3) ethanol solution is added into the precipitation containing tea saponin, 2 5h is leached in 60 70 DEG C under stirring, is separated off solid impurity, obtains the ethanol solution containing tea saponin；(4) ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；(5) pH value of extracting solution is adjusted to acidity, resting solution and Camellia nitidissima saponin extract is made through being concentrated in vacuo, being spray-dried.The yield of the present invention is high, does not pollute rapidly and efficiently, by extracting material.
Description
Technical field
The present invention relates to oil extraction technical field, and in particular to a kind of extraction process of Camellia nitidissima saponin extract.
Background technology
Camellia nitidissima [Camellia chrysantha (Hu) Tuyama] belongs to Theaceae, Camellia, Camellia Section Chrysantha.
Nineteen sixty finds first in Guangxi, due to its floral wax matter is golden yellow, golden valve jade stamen, the pretty cause of floridity, the famous plant in nineteen sixty-five China
Scholar Hu Xian doctors Jiasu are named as Camellia nitidissima.A kind of Camellia nitidissima plant resources rare as world (is only distributed in Guangxi
With one band of Vietnam border), local always by as Traditional Folk Chinese herbal medicine, for treating sphagitis, dysentery, hypertension, pre-
Preventing tumor, have blood in stool, [woods Hua Juan, waits food science and technologies, 2010,35 (10) to the disease such as irregular menstruation:88-91].By authoritative department and
Scientific research institution's detection shows that golden camellia tea contains more than 400 kinds of nutriment, rich in a variety of natural nutrition compositions.Golden camellia tea is institute
There is the general flavone content in tealeaves highest.Golden camellia tea is obvious because having containing active skull cap components such as abundant flavonoids
Slow down aging, improve immunity of organism, atherosclerosis, suppress tumour growth, reduce cholesterol, lowering blood pressure and blood fat
Deng effect.
Saponin(e is the more complicated glucoside compound of a class formation, is widely present in the category of nature section more than 90 more than 500
In plant.Tea saponin (also known as Tea Saponin) in cake of camellia oleifera seeds containing 10%-20%, tea saponin is a kind of pentacyclic triterpene glucoside
Compound, soluble easily in water, methanol, hydrous ethanol and n-butanol, are a kind of nonionic surfactants of function admirable, have compared with
The effect such as strong foaming, emulsification, scattered, moistening, and with the physiological activity such as impervious, anti-inflammatory, analgesia, anticancer, antimycotic, extensively
Applied to daily use chemicals, pesticide and other field, therefore there is higher economic value.
At present, a kind of extraction process of the high Camellia nitidissima saponin extract of yield is lacked.
The content of the invention
To solve the above problems, the shortcomings that the object of the present invention is to provide being to overcome the prior art, there is provided one kind production
The extraction process of the high Camellia nitidissima saponin extract of rate.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：A kind of golden flower tea saponins of the present invention carry
The extraction process of thing is taken, is included the following steps：
(1) golden camellia tea fragment is added to the water, and extracts 2-5h in 50-80 DEG C, then isolated Aqueous extracts and impurity；
Impurity is added to the water, 2-5h is extracted again in 50-80 DEG C, separates again, Aqueous extracts are made；Then by Aqueous extracts twice
Crude extract is made by initial gross separation, is then concentrated, then by purification with macroreticular resin, is eluted with solvent, receives
Collect eluent；
(2) precipitating reagent of its volume 1/5-1/10 is added into eluent, reacts 30-60min, Ran Houfen in 40-60 DEG C
From obtain lower floor generation the precipitation containing tea saponin；
(3) ethanol solution is added into the precipitation containing tea saponin, 2-5h is leached in 60-70 DEG C under stirring, is separated off
Solid impurity, obtains the ethanol solution containing tea saponin；
(4) ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；
(5) pH value of extracting solution is adjusted to acidity, through being concentrated in vacuo, being spray-dried, Camellia nitidissima saponin extract is made.
Further, in step (1), the solid-to-liquid ratio of the golden camellia tea and water is 1g/5ml；By golden flower to be extracted
Tea tealeaves cleans up；Golden camellia tea is subjected to microwave drying, golden camellia tea is crushed, is sieved with 40-60 mesh sieve, gold is made
Jasmine tea leaf fragment；The macroporous absorbent resin is low pole or nonpolar macroporous adsorption resin；The solvent is ethanol.
Further, in step (2), the rotating speed during separation is 3500-4000r/min, and separation lower sediment obtains
To the precipitation containing tea saponin.
Further, in step (2), the precipitating reagent is the modified cellulose that viscosity is 2000-4500mPas.
Further, in step (2), the modified cellulose is carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl
Any one in methylcellulose or methylcellulose.
Further, in step (3), the volumetric concentration of the ethanol solution is the ethanol solution of 70-90%.
Further, in step (3), in extraction, the precipitation containing tea saponin is added to the second of 3-8 times of its quality
In alcoholic solution；After the completion of extraction, filter and remove solid impurity, obtain the ethanol solution containing tea saponin.
Further, in step (4), it is described distillation recovery ethanol when, vapo(u)rizing temperature be 80-90 DEG C.
Further, in step (5), temperature during vacuum concentration is 50-80 DEG C, and temperature during spray drying is 80-
100℃。
Beneficial effect：The yield of the present invention is high, does not pollute rapidly and efficiently, by extracting material.Preparation process of the present invention is simple,
Reaction condition is gentle.
Compared with prior art, the present invention have the following advantages that：
(1) present invention, by macroreticular resin, avoids the interference of the components such as colloid, albumen, obtains using tea saponin as raw material
Theasapogenol purity it is high.
(2) present invention uses alkyd or alcohol alkali process, and theasapogenol structure is broken caused by can avoiding direct soda acid processing
It is bad, maintain its structural intergrity.
(3) modified cellulose that the present invention uses can be used as food additives, and safe and harmless, obtained tea saponin product is pure
It is good to spend better quality.
Embodiment
The present invention is further illustrated by the following examples.It should be understood that these embodiments are the explainations of the present invention
And citing, do not limit the scope of the invention in any form.
Embodiment 1
A kind of extraction process of Camellia nitidissima saponin extract of the present invention, includes the following steps：
(1) golden camellia tea to be extracted is cleaned up；Golden camellia tea fragment is added to the water, and extracts 2h in 50 DEG C, so
Isolated Aqueous extracts and impurity afterwards；Impurity is added to the water, 3h is extracted again in 80 DEG C, separates again, Aqueous extracts are made；
Then crude extract is made by initial gross separation in Aqueous extracts twice, is then concentrated, then pass through macroporous absorbent resin
Purifying, is eluted with solvent, collects eluent；The solid-to-liquid ratio of the golden camellia tea and water is 1g/5ml；Golden camellia tea is carried out micro-
Ripple is dried, and golden camellia tea is crushed, and is sieved with 40 mesh sieve, and golden camellia tea fragment is made；The macroporous absorbent resin is weak pole
Property macroporous absorbent resin；The solvent is ethanol.
(2) precipitating reagent of its volume 1/5 is added into eluent, reacts 60min in 60 DEG C, then isolated lower floor's life
Into the precipitation containing tea saponin；The rotating speed during separation is 3500r/min, and separation lower sediment is obtained containing tea saponin
Precipitation.The precipitating reagent is the modified cellulose that viscosity is 2000mPas.The modified cellulose is carboxymethyl cellulose.
(3) ethanol solution is added into the precipitation containing tea saponin, 4h is leached in 65 DEG C under stirring, it is miscellaneous to be separated off solid
Matter, obtains the ethanol solution containing tea saponin；The volumetric concentration of the ethanol solution is 80% ethanol solution.In extraction,
Precipitation containing tea saponin is added in the ethanol solution of 6 times of its quality；After the completion of extraction, filter and remove solid impurity, obtain
Ethanol solution containing tea saponin.
(4) ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；During the distillation recovery ethanol, steam
Temperature is evaporated for 86 DEG C.
(5) pH value of extracting solution is adjusted to acidity, resting solution and Camellia nitidissima soap is made through being concentrated in vacuo, being spray-dried
Glucoside extract.Temperature during vacuum concentration is 70 DEG C, and temperature during spray drying is 100 DEG C.
Embodiment 2
Embodiment 2 and embodiment 1 difference lies in：
A kind of extraction process of Camellia nitidissima saponin extract of the present invention, includes the following steps：
In step (1), golden camellia tea is subjected to microwave drying, golden camellia tea is crushed, sieved with 50 mesh sieve, is made
Golden camellia tea fragment.Golden camellia tea fragment is added to the water, and extracts 3h in 60 DEG C, then isolated Aqueous extracts and impurity；Will
Impurity is added to the water, and extracts 5h again in 60 DEG C, separates again；Merge separated Aqueous extracts；Then by Aqueous extracts twice
By macroporous absorbent resin, eluted with solvent, collect eluent；Golden camellia tea to be extracted is cleaned up；The macropore is inhaled
Attached resin is nonpolar macroporous adsorption resin；
In step (2), the precipitating reagent of its volume 1/10 is added into eluent, 50min is reacted in 40 DEG C, then separates
Obtain the precipitation containing tea saponin of lower floor's generation；The rotating speed during separation is 4000r/min, and separation lower sediment is contained
There is the precipitation of tea saponin.The precipitating reagent is the modified cellulose that viscosity is 3500mPas.The modified cellulose is hydroxyl second
Base cellulose.
In step (3), ethanol solution is added into the precipitation containing tea saponin, leaches 5h, separation under stirring in 60 DEG C
Solid impurity is removed, obtains the ethanol solution containing tea saponin；The volumetric concentration of the ethanol solution is 70% ethanol solution.
In extraction, the precipitation containing tea saponin is added in the ethanol solution of 8 times of its quality；After the completion of extraction, filter and remove solid
Impurity, obtains the ethanol solution containing tea saponin.
In step (4), the ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；The distillation recovery
During ethanol, vapo(u)rizing temperature is 90 DEG C.
In step (5), the pH value of extracting solution is adjusted to acidity, resting solution and is made through being concentrated in vacuo, being spray-dried
Camellia nitidissima saponin extract.Temperature during vacuum concentration is 80 DEG C, and temperature during spray drying is 80 DEG C.
Embodiment 3
Embodiment 3 and embodiment 1 difference lies in：
A kind of extraction process of Camellia nitidissima saponin extract of the present invention, includes the following steps：
In step (1), golden camellia tea is subjected to microwave drying, golden camellia tea is crushed, sieved with 60 mesh sieve, is made
Golden camellia tea fragment.Golden camellia tea fragment is added to the water, and extracts 5h in 80 DEG C, then isolated Aqueous extracts and impurity；Will
Impurity is added to the water, and extracts 2h again in 50 DEG C, separates again；Merge separated Aqueous extracts；Then by Aqueous extracts twice
By macroporous absorbent resin, eluted with solvent, collect eluent；Golden camellia tea to be extracted is cleaned up；
In step (2), the precipitating reagent of its volume 1/8 is added into eluent, 30min is reacted in 50 DEG C, then separates
Obtain the precipitation containing tea saponin of lower floor's generation；The rotating speed during separation is 3800r/min, and separation lower sediment is contained
There is the precipitation of tea saponin.The precipitating reagent is the modified cellulose that viscosity is 4500mPas.The modified cellulose is hydroxypropyl
Ylmethyl cellulose.
In step (3), ethanol solution is added into the precipitation containing tea saponin, leaches 2h, separation under stirring in 70 DEG C
Solid impurity is removed, obtains the ethanol solution containing tea saponin；The volumetric concentration of the ethanol solution is 90% ethanol solution.
In extraction, the precipitation containing tea saponin is added in the ethanol solution of 3 times of its quality；After the completion of extraction, filter and remove solid
Impurity, obtains the ethanol solution containing tea saponin.
In step (4), the ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；The distillation recovery
During ethanol, vapo(u)rizing temperature is 80 DEG C.
In step (5), the pH value of extracting solution is adjusted to acidity, resting solution and is made through being concentrated in vacuo, being spray-dried
Camellia nitidissima saponin extract.Temperature during vacuum concentration is 50 DEG C, and temperature during spray drying is 90 DEG C.
Embodiment 4
Embodiment 4 and embodiment 1 difference lies in：
In step (2), the modified cellulose is methylcellulose.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, the present invention
Claimed scope is delineated by the appended claims, the specification and equivalents thereof from the appended claims.
Claims (9)
1. a kind of extraction process of Camellia nitidissima saponin extract, it is characterised in that include the following steps：
(1) golden camellia tea fragment is added to the water, and extracts 2-5h in 50-80 DEG C, then isolated Aqueous extracts and impurity；Will be miscellaneous
Matter is added to the water, and extracts 2-5h again in 50-80 DEG C, separates again, and Aqueous extracts are made；Then Aqueous extracts twice are passed through
Crude extract is made in initial gross separation, is then concentrated, and then by purification with macroreticular resin, is eluted with solvent, collection is washed
De- liquid；
(2) precipitating reagent of its volume 1/5-1/10 is added into eluent, 30-60min is reacted in 40-60 DEG C, then separates
The precipitation containing tea saponin generated to lower floor；
(3) ethanol solution is added into the precipitation containing tea saponin, 2-5h is leached in 60-70 DEG C under stirring, is separated off solid
Impurity, obtains the ethanol solution containing tea saponin；
(4) ethanol solution containing tea saponin is distilled to recover ethanol, refluxing extraction；
(5) pH value of extracting solution is adjusted to acidity, through being concentrated in vacuo, being spray-dried, Camellia nitidissima saponin extract is made.
2. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (1), institute
The solid-to-liquid ratio for stating golden camellia tea and water is 1g/5ml；Golden camellia tea to be extracted is cleaned up；Golden camellia tea is subjected to microwave
It is dry, golden camellia tea is crushed, is sieved with 40-60 mesh sieve, golden camellia tea fragment is made；The macroporous absorbent resin is weak pole
Property or nonpolar macroporous adsorption resin；The solvent is ethanol.
3. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (2), institute
Rotating speed when stating separation is 3500-4000r/min, and separation lower sediment obtains the precipitation containing tea saponin.
4. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (2), institute
It is the modified cellulose that viscosity is 2000-4500mPas to state precipitating reagent.
5. the extraction process of Camellia nitidissima saponin extract according to claim 4, it is characterised in that：In step (2), institute
It is any in carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose or methylcellulose to state modified cellulose
It is a kind of.
6. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (3), institute
The volumetric concentration for stating ethanol solution is the ethanol solution of 70-90%.
7. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (3),
During extraction, the precipitation containing tea saponin is added in the ethanol solution of 3-8 times of its quality；After the completion of extraction, filter and remove solid
Impurity, obtains the ethanol solution containing tea saponin.
8. the extraction process of Camellia nitidissima saponin extract according to claim 1, it is characterised in that：In step (4), institute
When stating distillation recovery ethanol, vapo(u)rizing temperature is 80-90 DEG C.
9. according to the extraction process of claim 1 to 8 any one of them Camellia nitidissima saponin extract, it is characterised in that：In step
Suddenly in (5), temperature during vacuum concentration is 50-80 DEG C, and temperature during spray drying is 80-100 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929361A (en) * | 2018-08-30 | 2018-12-04 | 佛山市欧若拉生物科技有限公司 | A kind of processing technology of platycodin extract |
| CN111213754A (en) * | 2020-03-11 | 2020-06-02 | 广东仙塘红茶业有限公司 | Separation technology of alpine ancient tree tea saponin graphene and preparation technology of antioxidant buccal tablets |
| CN114903827A (en) * | 2022-05-07 | 2022-08-16 | 广东蒂姆森大健康科技有限公司 | Preparation method of high-stability Chinese honeylocust fruit aqueous extract |
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| CN102030804A (en) * | 2010-10-21 | 2011-04-27 | 华南理工大学 | Method for preparing theasapogenol |
| CN102731607A (en) * | 2012-06-25 | 2012-10-17 | 陕西科技大学 | Extraction and purification method of high-purity theasaponin |
| CN104262445A (en) * | 2014-09-01 | 2015-01-07 | 广西壮族自治区分析测试研究中心 | Camellia nitidissima saponin A, and preparation method and antitumor application thereof |
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| CN1071719A (en) * | 1991-10-24 | 1993-05-05 | 武汉大学 | The method for preparing scouring assistant with the tea cake |
| CN102030804A (en) * | 2010-10-21 | 2011-04-27 | 华南理工大学 | Method for preparing theasapogenol |
| CN102731607A (en) * | 2012-06-25 | 2012-10-17 | 陕西科技大学 | Extraction and purification method of high-purity theasaponin |
| CN104262445A (en) * | 2014-09-01 | 2015-01-07 | 广西壮族自治区分析测试研究中心 | Camellia nitidissima saponin A, and preparation method and antitumor application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108929361A (en) * | 2018-08-30 | 2018-12-04 | 佛山市欧若拉生物科技有限公司 | A kind of processing technology of platycodin extract |
| CN111213754A (en) * | 2020-03-11 | 2020-06-02 | 广东仙塘红茶业有限公司 | Separation technology of alpine ancient tree tea saponin graphene and preparation technology of antioxidant buccal tablets |
| CN114903827A (en) * | 2022-05-07 | 2022-08-16 | 广东蒂姆森大健康科技有限公司 | Preparation method of high-stability Chinese honeylocust fruit aqueous extract |
| CN114903827B (en) * | 2022-05-07 | 2023-11-28 | 广东蒂姆森大健康科技有限公司 | Preparation method of high-stability fructus gleditsiae water extract |
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