CN101962396A - Method for preparing tea saponin from oil tea cakes, tea seed meal, tea seed oil cakes - Google Patents
Method for preparing tea saponin from oil tea cakes, tea seed meal, tea seed oil cakes Download PDFInfo
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- CN101962396A CN101962396A CN2009101007702A CN200910100770A CN101962396A CN 101962396 A CN101962396 A CN 101962396A CN 2009101007702 A CN2009101007702 A CN 2009101007702A CN 200910100770 A CN200910100770 A CN 200910100770A CN 101962396 A CN101962396 A CN 101962396A
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- tea saponin
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- saponin
- oil
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- 241001122767 Theaceae Species 0.000 title claims abstract description 112
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 70
- 229930182490 saponin Natural products 0.000 title claims abstract description 70
- 150000007949 saponins Chemical class 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000010495 camellia oil Substances 0.000 title abstract description 6
- 239000003921 oil Substances 0.000 title abstract description 6
- 235000012054 meals Nutrition 0.000 title abstract 5
- 235000019198 oils Nutrition 0.000 title abstract 5
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012043 crude product Substances 0.000 claims description 24
- 241000209094 Oryza Species 0.000 claims description 17
- 235000007164 Oryza sativa Nutrition 0.000 claims description 17
- 235000009566 rice Nutrition 0.000 claims description 17
- 241000526900 Camellia oleifera Species 0.000 claims description 16
- 238000001953 recrystallisation Methods 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 235000015320 potassium carbonate Nutrition 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 230000037396 body weight Effects 0.000 claims description 2
- 238000010316 high energy milling Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000012046 mixed solvent Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 18
- 239000012153 distilled water Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 241000207199 Citrus Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- YKOPWPOFWMYZJZ-FMMUPTMQSA-N Echinocystic acid Natural products C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)C[C@H](O)[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C YKOPWPOFWMYZJZ-FMMUPTMQSA-N 0.000 description 1
- YKOPWPOFWMYZJZ-UHFFFAOYSA-N Echinocystsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CC(O)C5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C YKOPWPOFWMYZJZ-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940034982 antineoplastic agent Drugs 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- MCHWKJRTMPIHRA-UHFFFAOYSA-N n-(pyrrolidin-2-ylmethyl)aniline Chemical compound C1CCNC1CNC1=CC=CC=C1 MCHWKJRTMPIHRA-UHFFFAOYSA-N 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- -1 saponin sodium salt Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 150000008130 triterpenoid saponins Chemical class 0.000 description 1
- 229960005486 vaccine Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for preparing tea saponin from oil tea cakes, tea seed meal, tea seed oil cakes, which comprises the following steps: 1) drying the oil tea cakes, tea seed meal, tea seed oil cakes, feeding the oil tea cakes, tea seed meal, tea seed oil cakes into a high-energy grinding machine, adding a grinding assistant in an amount which is 1 to 20 percent based on the weight of the oil tea cakes, tea seed meal, tea seed oil cakes into the high-energy grinding machine for solid grinding; 2) adding water into the ground powder obtained by the step 1), stirring, extracting, filtering and mixing filtrate; 3) adding acid into the filtrate obtained by the step 2), crystallizing, precipitating, stirring, finishing crystallization and obtaining a coarse product of tea saponin; and 4) recrystallizing the coarse product of tea saponin obtained by the step 3) in aqueous ethanol-acetone mixed solvent in an amount which is 10 to 35 times the weight of the coarse product of tea saponin, and obtaining a fine product of the tea saponin. The method overcomes the drawbacks of low extraction rate, complex process equipment, high cost and difficult solvent recovery of the conventional method for extracting the tea saponin with an organic solvent. The method of the invention has the advantages of high extraction rate, simple process, small equipment investment, mild operation conditions, light environmental production and high product purity.
Description
Technical field
The present invention relates to tea seed industry deep processing and utilization field, relate in particular to a kind of method of from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered, producing tea saponin.
Background technology
Tea saponin is a kind of soap class of extracting from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered.Its basic structure is made up of triterpenoid saponin, structure sugar, structure acid.Pure tea saponin is oyster white or faint yellow solid amorphous powder, and fusing point is 223-224 ℃, and the average mark minor is C
57H
90O
26, relative molecular mass is 1200-2800.Tea saponin have foam low, acid low, diffusion is fast, easy cleaning, characteristics that volatilization is fast, is widely used in washing composition; That tea saponin has is impervious, anti-inflammatory, analgesia, anticancer, eliminate the phlegm, pharmacological function such as cough-relieving, be widely used in fields such as medicine industry pharmaceutical manufacturing, as preventing hypertension drug, anti-common mode agent, antineoplastic agent, penicillin additive, mad dog vaccine thinner, producing medicinal Echinocystic acid etc.; Tea saponin has multiple physiological actions such as sterilization, desinsection and promotion plant-growth, and its series pesticide agent, sterilant as the main raw material preparation can be used for the big area desinsection of citrus, paddy rice; Tea saponin can be used for the bubble stabilizer of gas concrete and steady bubble and gets angry etc.; Tea saponin also is used to aerating and mixes earth cast, metal cutting, tackiness agent, foam drilling, foaming water discharge etc., and performance obviously is better than other products.
Tea saponin generally adopts solvent-extraction process to produce at present, and extraction solvent commonly used has aqueous methanol, aqueous ethanol, propyl carbinol, water etc.Organic solvent extraction method processing unit is numerous and diverse, cost is high, and most organic solvent has toxicity, contaminate environment, and inflammable and explosive, there is production safety hidden danger; Traditional water formulation technology is simple, cost is low, less investment, instant effect, the tea saponin purity that but steam output is big, energy consumption is high, the production cycle is long and extract is low, color is dark, of poor quality, product mostly is slurry, the repurity difficulty, can only be used for agricultural chemicals, asphalt emulsifier, can not be applied to aspects such as makeup, solubilising, foaming, production reagent, unfavorable to the resources of tea saponin utilization with exploitation.
As mentioned above, the tea saponin method of producing in the background technology still has the some shortcomings part, the object of the present invention is to provide a kind of method of from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered, producing tea saponin, it is to utilize tea saponin to be slightly acidic, in high-energy mills, carry out solid state reaction and generate water miscible tea saponin sodium salt, sylvite or ammonium salt, get the tea saponin elaboration through flooding, acidifying, recrystallization with grinding aid.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of producing tea saponin from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered is provided.
The method of from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered, producing tea saponin be withered with cake of camellia oleifera seeds, the tea dregs of rice or tea be raw material, get tea saponin through pulverizing, high energy milling, flooding, acidifying, recrystallization, concrete steps are as follows:
1) with cake of camellia oleifera seeds, the tea dregs of rice or the withered raw material stoving of tea, pulverize, add in the high-energy mills, other gets the grinding aid of raw material weight 1～20%, and solid-state grinding is 15 minutes～3 hours in the adding high-energy mills;
2) get the grinding powder that step 1) makes, add the water of 5～50 times of lapping powder body weight, stir, filter 23～5 time, merging filtrate;
3) in step 2) add acid in the gained filtrate, crystallization is separated out, and stirs, and makes crystallization complete, the tea saponin crude product;
4) get step 3) gained tea saponin crude product, the solvent recrystallization that usefulness tea saponin crude product weight is 10～35 times 2～3 times gets the tea saponin elaboration.
Described grinding aid is one or more in yellow soda ash, sodium bicarbonate, sodium hydroxide, salt of wormwood, saleratus or potassium hydroxide or the ammonium chloride.Described high-energy mills is planetary ball mill, agitating ball mill or oscillating mill.Described acid is glacial acetic acid, hydrochloric acid or sulfuric acid.Described solvent is one or more in water, ethanol or the acetone.
The advantage that comparison had of the present invention and prior art is the extraction yield height, technology is simple, facility investment is few, operational condition is gentle, low in the pollution of the environment, the product purity height; Avoid use poisonous, inflammable and explosive organic solvent; The drawback of having avoided traditional water extraction method restriction tea saponin to be further purified.
Description of drawings
Accompanying drawing is the infrared spectrogram of embodiment 1 tea saponin.
Embodiment
The present invention is further described in conjunction with following example, but content of the present invention is not limited only to content related among the embodiment.
Embodiment 1
1) take by weighing 50 gram tea seed cakes, oven dry is pulverized, and other takes by weighing 0.5 gram yellow soda ash, adds in the lump in the PM100 type planetary ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 650 rev/mins, grinds 15 minutes;
2) get the grinding powder that step 1) makes, with 250 gram distilled water, stirring at room, filter 23, merging filtrate;
3) in step 2) add glacial acetic acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 4.9 restrains.
4) get step 3) gained tea saponin crude product, with 49 gram distilled water recrystallizations three times, the tea saponin elaboration, its infrared spectrogram is seen accompanying drawing.
Embodiment 2
1) take by weighing 100 gram leached tea oil slags, oven dry is pulverized, and other takes by weighing 10 gram sodium bicarbonates, adds in the 8000D-230 type high energy vibration shredder, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 600 rev/mins, grinds 180 minutes;
2) get the grinding powder that step 1) makes, with 500 gram distilled water, stirring at room is filtered merging filtrate 5 times;
3) in step 2) add hydrochloric acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 11.2 restrains.
4) get step 3) gained tea saponin crude product,, get the tea saponin elaboration with 224 gram alcohol crystal secondaries.
Embodiment 3
1) take by weighing the 100 gram oil tea dregs of rice, oven dry is pulverized, and other takes by weighing 15 gram sodium hydroxide, adds in the GSY-2 type agitating ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 500 rev/mins, grinds 120 minutes;
2) get the grinding powder that step 1) makes, with 1080 gram distilled water, stirring at room is filtered merging filtrate 4 times;
3) in step 2) add sulfuric acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 10.3 restrains.
4) get step 3) gained tea saponin crude product, with 103 gram ethyl alcohol recrystallizations three times, the tea saponin elaboration.
Embodiment 4
1) take by weighing 100 gram cake of camellia oleifera seeds, oven dry is pulverized, and other takes by weighing 18 gram salt of wormwood, adds in the AGO-2 type planetary ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 1290 rev/mins, grinds 60 minutes;
2) get the grinding powder that step 1) makes, with 2000 gram distilled water, stirring at room is filtered merging filtrate 5 times;
3) in step 2) add glacial acetic acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 9.9 restrains.
4) get step 3) gained tea saponin crude product, with 346.5 gram acetone recrystallizations three times, the tea saponin elaboration.
Embodiment 5
1) it is withered to take by weighing 100 gram tea, and oven dry is pulverized, and other takes by weighing 15 gram saleratus, adds in the AGO-2 type planetary ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 1290 rev/mins, grinds 120 minutes;
2) get the grinding powder that step 1) makes, with 2500 gram distilled water, stirring at room, filter 23, merging filtrate;
3) in step 2) add hydrochloric acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 11.4 restrains.
4) get step 3) gained tea saponin crude product, with 285 gram ethanol-acetone solvent recrystallization three times, the tea saponin elaboration.
Embodiment 6
1) it is withered to take by weighing 100 gram tea, and oven dry is pulverized, and other takes by weighing 10 gram potassium hydroxide, adds in the AGO-2 type planetary ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 1290 rev/mins, grinds 45 minutes;
2) get the grinding powder that step 1) makes, with 3500 gram distilled water, stirring at room is filtered merging filtrate 5 times;
3) in step 2) add sulfuric acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 11.5 restrains.
4) get step 3) gained tea saponin crude product, with 230 gram water-ethanol solvent recrystallization three times, the tea saponin elaboration.
Embodiment 7
1) it is withered to take by weighing 100 gram tea, and oven dry is pulverized, and other takes by weighing 13 gram ammonium chlorides, adds in the AGO-2 type planetary ball mill, and ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), and rotating speed is 1290 rev/mins, grinds 90 minutes;
2) get the grinding powder that step 1) makes, with 4000 gram distilled water, stirring at room is filtered merging filtrate 4 times;
3) in step 2) add glacial acetic acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 11.8 restrains.
4) get step 3) gained tea saponin crude product, with 118 gram water-acetone solvent recrystallization three times, the tea saponin elaboration.
Embodiment 8
1) it is withered to take by weighing 100 gram tea, and oven dry is pulverized, and other takes by weighing 12 gram yellow soda ash, 2 gram sodium bicarbonates, 1 gram salt of wormwood, add in the AGO-2 type planetary ball mill, ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), rotating speed is 1290 rev/mins, grinds 150 minutes;
2) get the grinding powder that step 1) makes, with 4500 gram distilled water, stirring at room, filter 23, merging filtrate;
3) in step 2) add glacial acetic acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 11.8 restrains.
4) get step 3) gained tea saponin crude product, with 236 gram aqueous ethanols-acetone double solvents recrystallization three times, the tea saponin elaboration.
Embodiment 9
1) take by weighing 100 gram tea seed cakes, oven dry is pulverized, and other takes by weighing sodium bicarbonate, salt of wormwood, each 1 gram of saleratus, salt of wormwood 15 grams, add in the AGO-2 type planetary ball mill, ball-milling medium is an agate ball, and medium and material ratio are 1: 1 (w/w), rotating speed is 1290 rev/mins, grinds 180 minutes;
2) get the grinding powder that step 1) makes, with 5000 gram distilled water, stirring at room is filtered merging filtrate 4 times;
3) in step 2) add sulfuric acid in the gained filtrate, stir, crystallization is separated out fully, tea saponin crude product 10.6 restrains.
4) get step 3) gained tea saponin crude product, with 180 gram moisture-ethanol-acetone solvent recrystallization three times, the tea saponin elaboration.
Claims (5)
1. method of from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered, producing tea saponin, it is characterized in that it be withered with cake of camellia oleifera seeds, the tea dregs of rice or tea be raw material, get tea saponin through pulverizing, high energy milling, flooding, acidifying, recrystallization, concrete steps are as follows:
1) with cake of camellia oleifera seeds, the tea dregs of rice or the withered raw material stoving of tea, pulverize, add in the high-energy mills, other gets the grinding aid of raw material weight 1～20%, and solid-state grinding is 15 minutes～3 hours in the adding high-energy mills;
2) get the grinding powder that step 1) makes, add the water of 5～50 times of lapping powder body weight, stir, filter 23～5 time, merging filtrate;
3) in step 2) add acid in the gained filtrate, crystallization is separated out, and stirs, and makes crystallization complete, the tea saponin crude product;
4) get step 3) gained tea saponin crude product, the solvent recrystallization that usefulness tea saponin crude product weight is 10～35 times 2～3 times gets the tea saponin elaboration.
2. a kind of method of producing tea saponin from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered as claimed in claim 1 is characterized in that described grinding aid is one or more in yellow soda ash, sodium bicarbonate, sodium hydroxide, salt of wormwood, saleratus or potassium hydroxide or the ammonium chloride.
3. a kind of method of producing tea saponin from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered as claimed in claim 1 is characterized in that described high-energy mills is planetary ball mill, agitating ball mill or oscillating mill.
4. a kind of method of producing tea saponin from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered as claimed in claim 3 is characterized in that described acid is glacial acetic acid, hydrochloric acid or sulfuric acid.
5. a kind of method of producing tea saponin from cake of camellia oleifera seeds, the tea dregs of rice or tea are withered as claimed in claim 4 is characterized in that described solvent is one or more in water, ethanol or the acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101007702A CN101962396B (en) | 2009-07-21 | 2009-07-21 | Method for preparing tea saponin from oil tea cakes, tea seed meal, tea seed oil cakes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101007702A CN101962396B (en) | 2009-07-21 | 2009-07-21 | Method for preparing tea saponin from oil tea cakes, tea seed meal, tea seed oil cakes |
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| Publication Number | Publication Date |
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| CN101962396A true CN101962396A (en) | 2011-02-02 |
| CN101962396B CN101962396B (en) | 2012-11-21 |
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Cited By (9)
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| CN102351922A (en) * | 2011-08-04 | 2012-02-15 | 浙江工业大学 | Method for extracting tea saponin from Camellia oleiera Aberl. cake |
| CN102533435A (en) * | 2012-01-19 | 2012-07-04 | 胡黎明 | Method for producing tea oil and tea seed cakes with tea dry cookies as raw materials |
| CN102690320A (en) * | 2012-05-24 | 2012-09-26 | 管天球 | Process for extracting tea cake protein and tea cake tea saponin in one time |
| CN103232500A (en) * | 2013-05-06 | 2013-08-07 | 福建农林大学 | Method for extracting tea saponin by adopting plant ash-quicklime precipitation |
| CN103275163A (en) * | 2013-05-23 | 2013-09-04 | 安徽省华银茶油有限公司 | Extraction method for promoting tea saponin to bleed out through surfactant |
| CN105175476A (en) * | 2015-09-02 | 2015-12-23 | 常州市长宇实用气体有限公司 | Method for extracting tea saponin from camellia oleifera abel cake meal |
| CN105418722A (en) * | 2015-11-12 | 2016-03-23 | 安徽农业大学 | Camellia saponin C4, C5 and C6 pentacyclic triterpenoid and preparation method and application thereof |
| CN108070015A (en) * | 2016-11-16 | 2018-05-25 | 江南大学 | A kind of method for recycling ethyl alcohol and Tea Saponin simultaneously from using the water phase after ethyl alcohol water extraction extract oil tea-seed oil |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1224022A (en) * | 1998-04-17 | 1999-07-28 | 重庆市协瑞科贸有限公司 | New process for extracting tea saponin |
| CN101440117A (en) * | 2008-12-30 | 2009-05-27 | 广东新大地生物科技股份有限公司 | Method for extracting tea saponin from tea cake |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351922A (en) * | 2011-08-04 | 2012-02-15 | 浙江工业大学 | Method for extracting tea saponin from Camellia oleiera Aberl. cake |
| CN102533435A (en) * | 2012-01-19 | 2012-07-04 | 胡黎明 | Method for producing tea oil and tea seed cakes with tea dry cookies as raw materials |
| CN102690320A (en) * | 2012-05-24 | 2012-09-26 | 管天球 | Process for extracting tea cake protein and tea cake tea saponin in one time |
| CN102690320B (en) * | 2012-05-24 | 2013-09-25 | 管天球 | Process for extracting tea cake protein and tea cake tea saponin in one time |
| CN103232500A (en) * | 2013-05-06 | 2013-08-07 | 福建农林大学 | Method for extracting tea saponin by adopting plant ash-quicklime precipitation |
| CN103275163A (en) * | 2013-05-23 | 2013-09-04 | 安徽省华银茶油有限公司 | Extraction method for promoting tea saponin to bleed out through surfactant |
| CN103275163B (en) * | 2013-05-23 | 2016-01-06 | 安徽省华银茶油有限公司 | The extracting method that tea saponin oozes out urged by a kind of tensio-active agent |
| CN105175476A (en) * | 2015-09-02 | 2015-12-23 | 常州市长宇实用气体有限公司 | Method for extracting tea saponin from camellia oleifera abel cake meal |
| CN105418722A (en) * | 2015-11-12 | 2016-03-23 | 安徽农业大学 | Camellia saponin C4, C5 and C6 pentacyclic triterpenoid and preparation method and application thereof |
| CN105418722B (en) * | 2015-11-12 | 2017-12-19 | 安徽农业大学 | A kind of entitled Sasanguasaponin C4And C5Pentacyclic triterpenoid preparation method |
| CN108070015A (en) * | 2016-11-16 | 2018-05-25 | 江南大学 | A kind of method for recycling ethyl alcohol and Tea Saponin simultaneously from using the water phase after ethyl alcohol water extraction extract oil tea-seed oil |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
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