CN102250681A - Method for extracting camellia oil and tea saporin from tea seeds - Google Patents

Method for extracting camellia oil and tea saporin from tea seeds Download PDF

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CN102250681A
CN102250681A CN2011101659027A CN201110165902A CN102250681A CN 102250681 A CN102250681 A CN 102250681A CN 2011101659027 A CN2011101659027 A CN 2011101659027A CN 201110165902 A CN201110165902 A CN 201110165902A CN 102250681 A CN102250681 A CN 102250681A
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water
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oil
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CN102250681B (en
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杨瑞金
张文斌
李强
华霄
赵伟
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Jiangnan University
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Abstract

The invention relates to a method for extracting camellia oil and tea saporin from tea seeds. The method provided by the invention comprises the following steps of: pre-treating tea seeds, extracting camellia oil in a water phase, extracting tea saporin, recycling a solvent and the like. The oil extracting rate obtained by using the method provided by the invention can be more than 95%, the recycling rate of the tea saporin is more than 85% and the oil quality of the camellia oil is good. In the method provided by the invention, ethanol or isopropanol is utilized as the solvent so that the camellia oil is safe and toxic, has a lower boiling point, is easily recycled and repeatedly utilized, can reduce manufacturing cost, is environmental-friendly and has a very wide application prospect.

Description

A kind of from tea seed the method for extract oil tea-seed oil and tea saponin
[technical field]
The invention belongs to the utilization of agricultural resources utilization technical field.More specifically, the present invention relates to a kind of from tea seed the method for extract oil tea-seed oil and tea saponin.
[background technology]
Oil tea (camellia oleifera) is Chinese distinctive oil crops.600,000 tons of tea seeds are produced in the whole nation per year, and wherein Hunan, Jiangxi provinces output account for more than 60% of national output.The tea saponin content of tea seed is about 8.0~12.0%, its oleaginousness is up to 35.0~60.0%, the lipid acid of camellia seed oil is formed similar to sweet oil, particularly oleic acid and linoleic content are up to more than 90%, and also contain multiple functional ingredient, have effects such as tangible prevention cardiovascula arteriosclerosis, hypotensive, reducing blood-fat, enormously potential as high-grade fry dried food ingredients exhibition.Tea saponin (tea saponin, TS), claim theasaponin, tea saponin again, it is a kind of nonionogenic tenside of excellent property, have stronger foaming, emulsification, dispersion, effect such as moistening, and have impervious, anti-inflammatory, analgesia, physiologically active such as anticancer, and can be widely used in industries such as food, medicine, daily use chemicals, agricultural chemicals, economic worth is higher.
The tea-seed oil extracting method mainly contains milling process and extraction.Milling process can keep the flavour of product, and the peanut oil of home sale generally is to adopt this production technique at present.But this method residual oil content height (7~10%), labour intensity is big, cost is high, power consumption is big, and protein denaturation is serious in the grouts, can only be used as fertilizer, causes the proteic waste of a large amount of quality plants.By comparison, lixiviation process production efficiency height and residual oil content low (1~4%).But lixiviation process also has weak point: equipment is many, investment is big; The crude oil complicated component needs strict refining treatment, and the oil product flavor loss is big; Wet dregs of rice sex change in high temperature precipitation process is big; For the high oilseed of oil length, adopt direct leaching solvent recovering system load big; With an organic solvent increased technology loaded down with trivial details property, reduced the security of producing, the pollution that has caused environment; Micro-organic solvent residual in the processed oil is unfavorable to human health.Pre-press for extracting juice-the lixiviation process that also has two kinds of methods to adopt simultaneously, soon 70~80% oil extrudes with milling process earlier in the raw material, more remaining oil is extracted with lixiviation process.Though the pre-lixiviation process oil extracting rate height (dregs of rice residual oil content is below 1%, and powder-material is below 2%) that presses is put forward oily process and is caused protein denaturation in various degree, thereby influence its nutritive value and functional property, and solvent extraction process need desolventizing, equipment is many, investment is big, pollutes heavy.By contrast, aqueous extraction method mild condition, equipment are simple, environmental friendliness, oil quality height, but because more easily cause that a large amount of emulsification causes the edible vegetable oil yield not high.
The extracting method of tea saponin mainly contains water extract method, organic solvent extraction etc.Wherein, production technique, the equipment of water extract method are simple, but produce a large amount of waste water and residue in process of production, the later separation difficulty, and product purity is low, and energy consumption is big.The organic solvent extraction method mainly is an alcohol extracting method, methanol extraction commonly used and extraction using alcohol, and because of methanol solvate is not only inflammable and explosive, boiling point is low, and toxicity is big, safety in production requires high.Water extraction and alcohol precipitation method is the improvement of water extraction and organic solvent method, has drawn both advantages.Water extraction impurity is many, purity is low, and aftertreatment is difficulty quite; Big, high, the complex process of cost of organic solvent method investment.Water extraction and alcohol precipitation method has overcome both weak points.
At present, reported that the research about extract grease and tea saponin from tea seed comprises: (forestry scientific research such as Fang Xuezhi, Wang Kailiang, Yao Xiaohua, 2010,10,23 (5): 778~781) utilize the aqueous enzymatic extraction tea-seed oil, compared the influence of the adding mode of different enzymes to the aqueous enzymatic method oil extracting process, this technology oil extracting rate is lower, only is 82.17%.The Zhang Weiguo of Shaoguan College (CN101569329) proposes use earlier the organic solvent extraction tea saponin, and back employing reduction vaporization has reclaimed organic solvent in the tea seed residue to carry out aqueous enzymatic method again and carry oil.This process synthesis utilization has also been reclaimed tea-seed oil and the tea saponin in the tea seed, and its oil extracting rate is 85%, and comparing early-stage Study has had certain improvement.
At present, both at home and abroad people (CN101569329) such as Zhang Weiguo proposes to utilize the grease that then adopts behind the tea saponin in the organic solvent extraction tea seed in the aqueous enzymatic extraction tea seed residue in the research, but carried out Recovery of Organic Solvent earlier and carry out next step Enzymatic Extraction again in technology, energy consumption is bigger.In addition, its total free oil yield only is 85%, also fails the tea seed resource is realized efficient the utilization.(Transactions of the Chinese Society of Agricultural Engineering, 2010,9 such as Guo Yubao, Tukon, Xue Zhenglian, 9 (26): 362~366) utilize the salts solution auxiliary water to extract tea-seed oil for method from tea seed, the edible vegetable oil yield is higher, reaches 96.33%, suitable with extraction, but very big with the salt amount, every 100g raw material need consume about 85gNa 2CO 3, used salt can't be recycled, and not only promotes cost and causes environmental pollution easily.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of from tea seed the method for extract oil tea-seed oil and tea saponin.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of from tea seed the method for extract oil tea-seed oil and tea saponin.
Steps A: camellia seed kernel after pulverizing mixes 1 parts by weight of crushed camellia seed kernel and 3~6 weight parts waters, adds 0.4~0.8 weight part alcoholic solution again and makes the concentration expressed in percentage by volume of final alcohol reach 10~25%, obtains camellia seed kernel pre-treatment mixture;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains with water extraction 0.5~2h, carries out centrifugation then under the condition of 40~70 ℃ of temperature and pH7~10, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 5~10 weight parts waters lixiviate 0.5~3h under the condition of 40~70 ℃ of temperature mutually, centrifugation obtains a kind of water and a kind of slag mutually then, and described slag repeats lixiviate 2-4 time in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, and add flocculation agent KAlSO then 4L2H 2O dissolves, mixes, and carries out centrifugation again and removes the contamination precipitation thing, and the water that centrifugation is collected carries out evaporation concentration or membrane concentration, obtains a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 3~5 volume ethanol solution in the concentrated solution that obtains, under 60~80 ℃ of temperature, carry out alcohol precipitation 1~3h, carry out centrifugation then, obtain a kind of water and a kind of slag mutually; Described slag returns step C mutually) continue to handle, and described water carries out evaporation concentration, reclaims ethanol, its residue drying obtains the tea saponin crude product.
A preferred embodiment of the invention, described camellia seed kernel grinding particle size is 60~200 orders.
According to another kind of preferred implementation of the present invention, in steps A) in, described alcohol is ethanol or Virahol.
According to another kind of preferred implementation of the present invention, at step B) in regulate the used alkali of pH and be selected from sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood or saleratus.
According to another kind of preferred implementation of the present invention, at step D) in, the consumption of described flocculation agent is with step B) and step C) all water weight of obtaining count 1.0%-2.0%.
According to another kind of preferred implementation of the present invention, in step e) in, described alcoholic acid concentration expressed in percentage by weight is 85~90%.
According to another kind of preferred implementation of the present invention, at step D) and E) in, under the condition of 100~110 ℃ of temperature and pressure 0.05~0.1MPa, carry out evaporation concentration.
Below the present invention will be described in more detail.
The present invention relates to a kind of from tea seed the method for extract oil tea-seed oil and tea saponin.
Technical solution of the present invention is as follows: shelling tea seed raw material is used the low-concentration ethanol extraction with aqueous solution after dry ground, carry out centrifugation then, and centrifugation obtains tea seed edible vegetable oil, water and tea seed residue mutually.The tea seed residue is used the flooding tea saponin mutually, repeats lixiviate 2-4 time, merges resulting all waters, adds flocculation agent and centrifugation again and removes impurity.The water that obtains adds the further precipitated impurities of ethanolic soln after concentrating.After the centrifugation, ethanol is reclaimed in evaporation to clear liquor, and makes the tea saponin crude product after the drying.
The step of this method is as follows:
Steps A: camellia seed kernel after pulverizing mixes 1 parts by weight of crushed camellia seed kernel and 3~6 weight parts waters, adds 0.4~0.8 weight part alcoholic solution again, and the concentration expressed in percentage by volume of described alcohol finally reaches 10~25%.
Use mechanical means that raw material powder is broken into 60~200 order pasty materials,, for example use in herbal medicine processing normally used pulverizer to carry out histocyte and destroy tea seed raw tissue cytoclasis.Preferably, the granularity of pulverizing camellia seed kernel is 80~160 orders, more preferably 100~140 orders.The contriver observes, and does not add water and can avoid forming stable milk sap in camellia seed kernel raw material pulverizing process in shattering process.
According to the present invention, described alcohol should be appreciated that it is a kind of alcoholic solvent that the solvable compositions of camellia seed kernel such as camellia seed oil in the pulverizing camellia seed kernel and tea saponin can be extracted.Therefore, every have this character and bring the alcoholic solvent of disadvantageous effect for again these stripping compositions, technological process or environment, may be used to the present invention.
In steps A of the present invention) in, described alcohol is ethanol or Virahol.Preferably, described alcohol is ethanol.
The inventor finds that if the final volume percentage concentration of described alcohol is lower than 10%, then demulsification is obvious inadequately, and oil extracting rate is lower; If the final volume percentage concentration of described alcohol is higher than 25%, then oil extracting rate is very slow with the concentration rising, is the difficulty that reduces alcoholic acid consumption and recovery, and it is 10~25% that the inventor has selected the final volume percentage concentration of described alcohol.
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains with water extraction 0.5~2h, carries out centrifugation then under the condition of 40~70 ℃ of temperature and pH7~10, obtain tea-seed oil phase, water and tea seed residue mutually.
In the extraction process by water of conventional grease, wrapped up by protein film by oily corpusculum in the seed oil tea seed kernel cell, and phosphatide and protein easily cause emulsification in process of lapping, can obtain the different oil in water emulsion of emulsification degree, so breakdown of emulsion are important steps of extraction process by water.In the present invention, different with traditional extraction process by water, the emulsus liquid phase that method of the present invention produced is thin especially, even does not almost have, and therefore improves the yield of tea-seed oil edible vegetable oil widely.Those skilled in the art know, alcohols is a kind of chemical demulsifier, alcohol can reduce the viscosity and the interfacial tension of its reaction system in this reaction system, change the type and the interfacial property of milk sap, has the character that reduces the liquid-solid interface film toughness or destroy its interfacial film, make the milk sap instability or be difficult to form milk sap, produced good demulsification, so improved tea-seed oil edible vegetable oil yield.A large amount of alcohol that described water contains not only can reduce emulsion, but also in addition recycling use reduces the pollution to environment, significantly cuts down finished cost.
When described camellia seed kernel pre-treatment mixture was used water extraction, it is bigger to the influence of extracting the tea-seed oil phase that it extracts temperature.Be lower than 40 ℃ if extract temperature, then oil extracting rate is lower.Be higher than 70 ℃ if extract temperature, then oil extracting rate no longer continues to rise, and Oxidation of Fat and Oils or hydrolysis risk increase.Therefore, take all factors into consideration energy consumption, oil quality and oil extracting rate, the described camellia seed kernel pre-treatment of present method mixture during with water extraction selected temperature be 40~70 ℃.
Similarly, when described camellia seed kernel pre-treatment mixture was used water extraction, its pH that extracts medium was bigger to the influence of extracting the tea-seed oil phase.Be lower than 7 or be higher than 10 if extract the pH of medium, then oil extracting rate is lower.Therefore, preferably, described camellia seed kernel pre-treatment mixture during with water extraction the pH of selected medium be 7~10.
More preferably, described camellia seed kernel pre-treatment mixture extracts 0.8~1.5h with ethanolic soln under the condition of 45~65 ℃ of temperature and pH 7.5~9.5.
Most preferably, described camellia seed kernel pre-treatment mixture extracts 1.0~1.2h with ethanolic soln under the condition of 50~60 ℃ of temperature and pH8.0~9.0.
In this step, the employed alkali of control pH is selected from sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood or saleratus.
In the present invention, employed equipment is normally used at the equipment of selling in the market in grease processing technology when described water extraction, for example goes up the thermostat water bath that the grand experimental installation of Nereid company limited sells.
In the present invention, described centrifugation is the separation of carrying out under rotating speed 1500-5000 rev/min condition.It is normally used at the whizzer of selling in the market in grease processing technology that the inventive method is carried out the employed whizzer of centrifugation, for example the whizzer of Shanghai medical analytical instrument factory sale.
Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil.For example those skilled in the art can form and the variation of some physical and chemical indexs according to the lipid acid of tea-seed oil in each refining procedure usually, be easy to determine its preferable machined parameters, as machined parameters such as alkali refining temperature, concentration of lye, bleaching temperature, bleaching times.
Step C:1 weight part is at step B) the tea seed residue that obtains uses 5~10 weight parts waters lixiviate 0.5~3h under the condition of 40~70 ℃ of temperature mutually, centrifugation obtains a kind of water and a kind of slag mutually then, and described slag repeats lixiviate 2-4 time in the mode mutually identical with described tea seed residue mutually again.
Preferably, described tea seed residue is used water extraction 1.0~2.5h under the condition of 45~65 ℃ of temperature.
More preferably, described tea seed residue is used water extraction 1.5~2.0h under the condition of 50~60 ℃ of temperature.
Water extraction equipment that this step is used and centrifugal separation equipment with at step B) in the equipment of use identical, also can use different equipment, but they all are normally used at the equipment of sale in the market in grease processing technology.
Step D: with step B) and step C) all waters of obtaining merge, and add flocculation agent KAlSO then 412H 2O dissolves, mixes, and carries out centrifugation again and removes the contamination precipitation thing, and the water that centrifugation is collected carries out evaporation concentration or membrane concentration, obtains a kind of concentrated solution.
In the present invention, described flocculation agent KAlSO 412H 2O (alum) is the water purification agent of using always, also is normally used in the grease processing technology.
The consumption of described flocculation agent is with step B) and step C) all water weight of obtaining count 0.1~2.0%, preferably 0.4~1.6%, more preferably 0.8~1.2%.
Described flocculation agent KAlSO 412H 2The granularity of O and adding mode are not very crucial, and those skilled in the art can be easy to determine the granularity and the adding mode of its flocculation agent as the case may be.
Equipment that this step is used and centrifugal separation equipment with at step B) in the equipment of use identical, also can use different equipment, but they all are normally used at the equipment of sale in the market in grease processing technology.
Step e: toward 1 weight part at step D) add 3~5 volume ethanol solution in the concentrated solution that obtains, under 60~80 ℃ of temperature, carry out alcohol precipitation 1~3h, carry out centrifugation then, obtain a kind of water and a kind of slag mutually; Described slag returns step C mutually) continue to handle, and described water carries out evaporation concentration, reclaims ethanol, its residue drying obtains the tea saponin crude product.
Adopted water extraction and alcohol precipitation method in the inventive method.Water extraction and alcohol precipitation method means that tea-seed oil benevolence adds flooding, extracts effective constituent such as tea-seed oil, organic acid, amino acid, polyose etc.; Also extract simultaneously some water-soluble impurities, as starch, protein, pigment, inorganic salt etc., in vat liquor, add ethanolic soln then, change the character of its vat liquor, reduce the solubility property of these various impurity, thereby make these contamination precipitations and be removed.
Preferably, toward 1 weight part at step D) add 3.2~4.8 volume ethanol solution in the concentrated solution that obtains, under 64~75 ℃ of temperature, carry out alcohol precipitation 1.5~2.5h.
More preferably, toward 1 weight part at step D) add 3.4~4.6 volume ethanol solution in the concentrated solution that obtains, under 68~70 ℃ of temperature, carry out alcohol precipitation 1.8~2.2h.
Concentration expressed in percentage by weight at the employed ethanolic soln of this step is 80~95%.
Described water carries out evaporation concentration, reclaims ethanol, and its residue drying obtains the tea saponin crude product.
At step D of the present invention) and E) in, under the condition of 100~110 ℃ of temperature and pressure 0.01~0.1MPa, carry out evaporation concentration.
The evaporation concentration equipment that uses in this two each and every one step all is normally used at the equipment of selling in the market, for example Rotary Evaporators of Taikan, Xi'an biotechnology group sale in grease processing technology.
In the present invention, the tea saponin content of resultant tea saponin crude product is to count 35~56% with tea saponin crude product gross weight.
Adopt the analytical procedure of resulting tea-seed oil of the inventive method and tea saponin crude product as follows:
The determination of fat method is Soxhlet extraction process (GB/T 5009.6-2003) in tea-seed oil.
Tea saponin Determination on content method is the Vanillin sulfuric acid process in the tea saponin crude product, and this method is the basic skills of tea saponin assay.
Lipid content and the tea saponin cubage oil extracting rate (edible vegetable oil yield) and the tea saponin rate of recovery that can obtain by mensuration according to following formula.
Oil extracting rate is defined as follows:
Figure BDA0000069424300000081
The tea saponin rate of recovery is defined as follows:
Figure BDA0000069424300000082
[beneficial effect]
Method of the present invention has following beneficial effect:
(1) handle in conjunction with water method and alcoholic solution, can improve the oil extracting rate of tea-seed oil effectively, oil extracting rate of the present invention can reach more than 95%, reclaims the fat in the raw material to greatest extent, improves the economy of technology.
(2) when improving the tea-seed oil extraction yield, the tea saponin in the energy efficient recovery raw material, the rate of recovery of tea saponin reaches more than 85%, reaches the purpose of comprehensive utilization tea seed.
(3) alcohol that adopts in the whole technological process is ethanol or Virahol, safety non-toxic, and boiling point is lower, is easy to recycle and reuse, and can reduce production costs environmental friendliness.
(4) the tea-seed oil oil quality that adopts the water method to extract is good.
(5) whole technological process is simple to operate, no complex apparatus, and equipment used is general-purpose equipment, and less input.
[description of drawings]
Fig. 1 represents to fully utilize the technical process that tea seed extracts tea-seed oil and tea saponin.
[embodiment]
To illustrate in greater detail the present invention by embodiment below.
Embodiment 1: adopt method of the present invention to extract tea-seed oil and tea saponin
This method implementation process as shown in Figure 1, concrete implementation step is as follows:
Steps A: purchase after the camellia seed kernel that obtains after the tea seed shelling of emblem, Anhui Camellia oil company limited is pulverized, obtaining granularity is 150 purpose materials, 1 parts by weight of crushed camellia seed kernel and 4 weight parts waters are mixed, add 0.5 weight part, 95% alcoholic solution again, mixing obtains camellia seed kernel pre-treatment mixture under the condition of 50 ℃ of temperature and stirring velocity 70rpm;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains uses the 1N sodium hydroxide solution with its pH regulator to 8, under the condition of 40 ℃ of temperature, use water extraction 1h then, carry out centrifugation with rotating speed 2500rpm again, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 9 weight parts waters lixiviate 3h under the condition of 50 ℃ of temperature mutually, obtain a kind of water and a kind of slag mutually with rotating speed 4000rpm centrifugation then, described slag repeats lixiviate 2 times in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, add then to merge water weight 0.1% flocculation agent KAlSO 412H 2O dissolving, mix, carry out centrifugation with rotating speed 3000rpm again and remove the contamination precipitation thing, the water that centrifugation is collected carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, obtain a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 4 volume 80% ethanolic solns in the concentrated solution that obtains, under 60 ℃ of temperature, carry out alcohol precipitation 1h, carry out centrifugation with rotating speed 3000rpm then, obtain a kind of water and a kind of slag mutually; Described water carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, reclaim ethanol, and its residue drying obtains the tea saponin crude product.
Obtaining oil extracting rate according to the measuring method of describing in the specification sheets and method of calculation is 95.45%, and the rate of recovery of tea saponin is 85.91%.
Embodiment 2: adopt method of the present invention to extract tea-seed oil and tea saponin
This method implementation step is as follows:
Steps A: purchase after the camellia seed kernel that obtains after the tea seed shelling of emblem, Anhui Camellia oil company limited is pulverized, obtaining granularity is 200 purpose materials, 1 parts by weight of crushed camellia seed kernel and 4 weight parts waters are mixed, add 0.8 weight part, 95% alcoholic solution again, mixing obtains camellia seed kernel pre-treatment mixture under the condition of 60 ℃ of temperature and stirring velocity 80rpm;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains uses the 1N aqueous sodium carbonate with its pH regulator to 9, under the condition of 50 ℃ of temperature, use water extraction 2h then, carry out centrifugation with rotating speed 4000rpm again, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 5 weight parts waters lixiviate 2h under the condition of 40 ℃ of temperature mutually, obtain a kind of water and a kind of slag mutually with rotating speed 4000rpm centrifugation then, described slag repeats lixiviate 3 times in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, add then to merge water weight 1% flocculation agent KAlSO 412H 2O dissolving, mix, carry out centrifugation with rotating speed 4000rpm again and remove the contamination precipitation thing, the water that centrifugation is collected carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, obtain a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 5 volume 85% ethanolic solns in the concentrated solution that obtains, under 65 ℃ of temperature, carry out alcohol precipitation 2h, carry out centrifugation with rotating speed 4000rpm then, obtain a kind of water and a kind of slag mutually; Described water carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, reclaim ethanol, and its residue drying obtains the tea saponin crude product.
Obtaining oil extracting rate according to the measuring method of describing in the specification sheets and method of calculation is 96.25%, and the rate of recovery of tea saponin is 85.68%.
Embodiment 3: adopt method of the present invention to extract tea-seed oil and tea saponin
This method implementation step is as follows:
Steps A: purchase after the camellia seed kernel that obtains after the tea seed shelling of emblem, Anhui Camellia oil company limited is pulverized, obtaining granularity is 100 purpose materials, 1 parts by weight of crushed camellia seed kernel and 3 weight parts waters are mixed, add 0.4 weight part, 95% alcoholic solution again, mixing obtains camellia seed kernel pre-treatment mixture under the condition of 50 ℃ of temperature and stirring velocity 70rpm;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains uses the 1N aqueous sodium hydroxide solution with its pH regulator to 7, under the condition of 60 ℃ of temperature, use water extraction 0.5h then, carry out centrifugation with rotating speed 1500rpm again, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 6 weight parts waters lixiviate 0.5h under the condition of 60 ℃ of temperature mutually, obtain a kind of water and a kind of slag mutually with rotating speed 3000rpm centrifugation then, described slag repeats lixiviate 4 times in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, add then to merge water weight 1.0% flocculation agent KAlSO 412H 2O dissolving, mix, carry out centrifugation with rotating speed 1500rpm again and remove the contamination precipitation thing, the water that centrifugation is collected carries out evaporation concentration or membrane concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, obtain a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 3 volume 95% ethanolic solns in the concentrated solution that obtains, under 80 ℃ of temperature, carry out alcohol precipitation 3h, carry out centrifugation with rotating speed 1500rpm then, obtain a kind of water and a kind of slag mutually; Described water carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, reclaim ethanol, and its residue drying obtains the tea saponin crude product.
Obtaining oil extracting rate according to the measuring method of describing in the specification sheets and method of calculation is 96.05%, and the rate of recovery of tea saponin is 88.11%.
Embodiment 4: adopt method of the present invention to extract tea-seed oil and tea saponin
This method implementation step is as follows:
Steps A: purchase after the camellia seed kernel that obtains after the tea seed shelling of emblem, Anhui Camellia oil company limited is pulverized, obtaining granularity is 60 purpose materials, 1 parts by weight of crushed camellia seed kernel and 5 weight parts waters are mixed, add 0.6 weight part, 95% alcoholic solution again, mixing obtains camellia seed kernel pre-treatment mixture under the condition of 60 ℃ of temperature and stirring velocity 80rpm;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains uses the 1N aqueous sodium carbonate with its pH regulator to 10, under the condition of 70 ℃ of temperature, use water extraction 1.5h then, carry out centrifugation with rotating speed 5000rpm again, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 10 weight parts waters lixiviate 1h under the condition of 70 ℃ of temperature mutually, obtain a kind of water and a kind of slag mutually with rotating speed 5000rpm centrifugation then, described slag repeats lixiviate 2 times in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, add then to merge water weight 1.0% flocculation agent KAlSO 412H 2O dissolving, mix, carry out centrifugation with rotating speed 5000rpm again and remove the contamination precipitation thing, the water that centrifugation is collected carries out evaporation concentration or membrane concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, obtain a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 4 volume 95% ethanolic solns in the concentrated solution that obtains, under 70 ℃ of temperature, carry out alcohol precipitation 2h, carry out centrifugation with rotating speed 5000rpm then, obtain a kind of water and a kind of slag mutually; Described water carries out evaporation concentration under the condition of 105 ℃ of temperature and pressure 0.05MPa, reclaim ethanol, and its residue drying obtains the tea saponin crude product.
Obtaining oil extracting rate according to the measuring method of describing in the specification sheets and method of calculation is 95.95%, and the rate of recovery of tea saponin is 85.01%.

Claims (7)

1. the method for extract oil tea-seed oil and tea saponin from a camellia seed kernel is characterized in that the step of this method is as follows:
Steps A: camellia seed kernel after pulverizing mixes 1 parts by weight of crushed camellia seed kernel and 3~6 weight parts waters, adds 0.4~0.8 weight part alcoholic solution again and makes the concentration expressed in percentage by volume of described alcohol finally reach 10~25%, obtains camellia seed kernel pre-treatment mixture;
Step B: the camellia seed kernel pre-treatment mixture that steps A) obtains with water extraction 0.5~2h, carries out centrifugation then under the condition of 40~70 ℃ of temperature and pH7~10, obtain tea-seed oil phase, water and tea seed residue mutually; Described tea-seed oil adopts the ordinary method of grease processing to handle mutually and obtains a kind of tea-seed oil;
Step C:1 weight part is at step B) the tea seed residue that obtains uses 5~10 weight parts waters lixiviate 0.5~3h under the condition of 40~70 ℃ of temperature mutually, centrifugation obtains a kind of water and a kind of slag mutually then, and described slag repeats lixiviate 2-4 time in the mode mutually identical with described tea seed residue mutually again;
Step D: with step B) and step C) all waters of obtaining merge, and add flocculation agent KAlSO then 412H 2O dissolves, mixes, and carries out centrifugation again and removes the contamination precipitation thing, and the water that centrifugation is collected carries out evaporation concentration or membrane concentration, obtains a kind of concentrated solution;
Step e: toward 1 weight part at step D) add 3~5 volume ethanol solution in the concentrated solution that obtains, under 60~80 ℃ of temperature, carry out alcohol precipitation 1~3h, carry out centrifugation then, obtain a kind of water and a kind of slag mutually; Described slag returns step C mutually) continue to handle or abandon as waste, and described water carries out evaporation concentration, reclaims ethanol, its residue drying obtains the tea saponin crude product.
2. method according to claim 1 is characterized in that described camellia seed kernel grinding particle size is 60~200 orders.
3. method according to claim 1 is characterized in that in steps A) in, described alcohol is ethanol or Virahol.
4. method according to claim 1 is characterized in that at step B) in regulate the used alkali of pH and be selected from sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood or saleratus.
5. method according to claim 1 is characterized in that at step D) in, the consumption of described flocculation agent is with step B) and step C) all water weight of obtaining count 0.1~2.0%.
6. method according to claim 1 is characterized in that in step e) in, the used ethanol concentration expressed in percentage by weight of alcohol precipitation is 80~95%.
7. method according to claim 1 is characterized in that at step D) and E) in, under the temperature 100-110 ℃ of condition with pressure 0.01~0.1MPa, carry out evaporation concentration.
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