Summary of the invention
The technical problem that present invention mainly solves: occur during extracting for conventional tea Saponin, water seaoning is extracted
Time the yield of tea saponin and purity low, limit the range of application of tea saponin, and during organic solvent extraction, methanol used be poisonous,
Though increasing with ethanol extraction purity relatively water extraction, but it is unable to reach high-purity problem, it is provided that a kind of from camellia seed meal
The method extracting tea saponin, the present invention is with camellia seed meal as raw material, after crushed, extracts defat by ethyl acetate, then uses at enzyme
Reason so that it is intracellular effective ingredient fully discharges, coordinates supersound extraction, recycling carbamide to coordinate dry ice cooling with ethanol subsequently,
Recrystallization, makes tea saponin precipitate, and is finally heated by precipitate, makes residual ethanol volatilize, and carbamide decomposes, and finally gives high-purity tea
Saponin solid.Gained tea saponin organic solvent-free of the present invention remains, and can completely decompose, taken out of by nitrogen stream after Urea, institute
Obtain tea saponin purity up to more than 98%.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weigh 200~300g camellia seed meals, be placed on stone grinder mill and pulverize, collect 80~100 mesh camellia seed meals
Powder, proceeds to fill in the Soxhlet extractor of 1~3L ethyl acetate, under the conditions of 75~80 DEG C, extracts 1~2h, and sucking filtration removes
Filtrate, is placed in gained filter cake in 60~65 DEG C of baking ovens, dried 2~4h, obtains defat camellia seed meal powder;
(2) weigh 30~50g above-mentioned gained defat camellia seed meal powder, add the beaker filling 100~200mL deionized waters
In, add 2~4g cellulase and 2~4g pectases, subsequently beaker is placed in digital display and tests the speed in constant temperature blender with magnetic force, add
Heat is warming up to 45~50 DEG C, and regulation rotating speed, to 300~400r/min, after stirring reaction 30~50min, is heated to 80~85
DEG C, adding 200~300mL mass concentrations is 70~80% ethanol solution, then proceeds to beaker, in sonic oscillation instrument, regulate ultrasonic
Frequency to 25~35kHz, oscillation treatment 10~20min, the mixed liquor in beaker is proceeded to centrifuge, centrifugation, takes supernatant
Liquid;
(3) in conical flask, adding 60~80mL above-mentioned gained supernatant, dropping mass concentration is 12~15% aqueous solution of urea,
Regulation pH value of solution, to 8.0~8.2, sprays conical flask surface 20~30s, centrifugation with liquid nitrogen subsequently, collects under first separation
Layer precipitate, proceeded in beaker, and collected supernatant, proceeded in conical flask, continue dropping mass concentration be 12~15% urine
Element aqueous solution, regulates pH to 8.3~8.5, sprays conical flask surface 35~45s, centrifugation with dry ice subsequently, collect secondary and divide
From lower sediment thing, it is merged with first separation precipitate, and collects supernatant, proceed in conical flask, continue dropping quality
Concentration is 12~15% aqueous solution of urea, regulates pH to 8.6~8.8, sprays conical flask surface 50~60s with dry ice subsequently, centrifugal
Separate, remove supernatant, collects three times separation lower sediment things, by its with once merge with secondary separation precipitate;
(4) above-mentioned gained sediment separate out is proceeded in tube type resistance furnace, in resistance furnace, be passed through nitrogen with 3~5mL/min speed
Gas shielded, is subsequently heated and is warming up to 160~180 DEG C, and heat treated 30~40min, under nitrogen guard mode, cools to the furnace
Room temperature, obtains tea saponin.
The concrete application process of the present invention: weigh 3~5g gained tea saponins of the present invention, be dissolved in 100~120mL deionized waters
In, it is configured to solution, subsequently solution is heated to 50~55 DEG C, put into 10~15g raw wools, immersion treatment 3~5min,
Per minute stir once, wash in the same way 3~5 times, finally solution is squeezed gently and go, proceed in 95~105 DEG C of baking ovens, dry
Dry to constant weight, with filter paper, dried Pilus Caprae seu Ovis is spooled subsequently, put in apparatus,Soxhlet's, add 100~120mL ether,
Under the conditions of 70~75 DEG C, extraction 20~30min, discharging, proceed to Pilus Caprae seu Ovis, in 95~105 DEG C of baking ovens, be dried to constant weight, after process
Pilus Caprae seu Ovis color and luster pure white, feel is fluffy soft and smooth, after testing, residual oils and fats rate be only 0.2~0.5%, more conventional Pilus Caprae seu Ovis emulsifying agent carries
High by more than 50%.
Beneficial effects of the present invention:
(1) camellia seed meal after the present invention utilizes oil-producing is raw material, improves the value of camellia seed meal, increases receipts for peasant
Enter source;
(2) present invention process short flow, improves the extraction ratio of tea saponin, and purity is up to more than 98%, improve tea soap
The range of application of element, has wide market application foreground.
Detailed description of the invention:
Weigh 200~300g camellia seed meals, be placed on stone grinder mill and pulverize, collect 80~100 mesh camellia seed meal powder
End, proceeds to fill in the Soxhlet extractor of 1~3L ethyl acetate, under the conditions of 75~80 DEG C, extracts 1~2h, and sucking filtration removes filter
Liquid, is placed in gained filter cake in 60~65 DEG C of baking ovens, dried 2~4h, obtains defat camellia seed meal powder;Weigh 30~50g
Above-mentioned gained defat camellia seed meal powder, adds in the beaker filling 100~200mL deionized waters, adds 2~4g celluloses
Enzyme and 2~4g pectases, be placed in beaker digital display subsequently and test the speed in constant temperature blender with magnetic force, be heated to 45~50 DEG C, adjusts
Joint rotating speed, to 300~400r/min, after stirring reaction 30~50min, is heated to 80~85 DEG C, adds 200~300mL matter
Amount concentration is 70~80% ethanol solution, then is proceeded to by beaker in sonic oscillation instrument, regulation supersonic frequency to 25~35kHz, vibration
Process 10~20min, the mixed liquor in beaker is proceeded to centrifuge, centrifugation, takes supernatant;In conical flask, add 60
~80mL above-mentioned gained supernatant, dropping mass concentration is 12~15% aqueous solution of urea, regulation pH value of solution to 8.0~8.2, with
Spray conical flask surface 20~30s, centrifugation with liquid nitrogen afterwards, collect first separation lower sediment thing, proceeded in beaker,
And collect supernatant, proceed in conical flask, continuing dropping mass concentration is 12~15% aqueous solution of urea, regulation pH to 8.3~
8.5, spray conical flask surface 35~45s, centrifugation with dry ice subsequently, collect secondary separation lower sediment thing, by it with one
Secondary sediment separate out merges, and collects supernatant, proceeds in conical flask, continue dropping mass concentration be 12~15% carbamide water-soluble
Liquid, regulates pH to 8.6~8.8, sprays conical flask surface 50~60s, centrifugation with dry ice subsequently, remove supernatant, collect
Three times separate lower sediment things, by its with once merge with secondary separation precipitate;Above-mentioned gained sediment separate out is proceeded to pipe
In formula resistance furnace, in resistance furnace, it is passed through nitrogen protection with 3~5mL/min speed, is subsequently heated and is warming up to 160~180 DEG C, add
Heat treatment 30~40min, under nitrogen guard mode, cools to room temperature with the furnace, obtains tea saponin.
Example 1
Weigh 200g camellia seed meal, be placed on stone grinder mill and pulverize, collect 80 mesh camellia seed meal powder, proceed to fill
In the Soxhlet extractor of 1L ethyl acetate, under the conditions of 75 DEG C, extracting 1h, sucking filtration removes filtrate, and gained filter cake is placed in 60 DEG C
In baking oven, dried 2h, obtain defat camellia seed meal powder;Weighing 30g above-mentioned gained defat camellia seed meal powder, addition fills
In the beaker of 100mL deionized water, add 2g cellulase and 2g pectase, subsequently beaker is placed in digital display and tests the speed constant temperature magnetic
On power agitator, it is heated to 45 DEG C, regulation rotating speed to 300r/min, after stirring reaction 30min, it is heated to 80 DEG C,
Adding 200mL mass concentration is 70% ethanol solution, then is proceeded to by beaker in sonic oscillation instrument, regulation supersonic frequency to 25kHz,
Oscillation treatment 10min, proceeds to centrifuge, centrifugation by the mixed liquor in beaker, takes supernatant;In conical flask, add
60mL above-mentioned gained supernatant, dropping mass concentration is 12% aqueous solution of urea, and regulation pH value of solution, to 8.0, sprays with liquid nitrogen subsequently
Conical flask surface 20s, centrifugation, collect first separation lower sediment thing, proceeded in beaker, and collect supernatant, turn
Entering in conical flask, continuing dropping mass concentration is 12% aqueous solution of urea, regulates pH to 8.3, sprays conical flask table with dry ice subsequently
Face 35s, centrifugation, collect secondary separation lower sediment thing, it is merged with first separation precipitate, and collects supernatant,
Proceeding in conical flask, continuing dropping mass concentration is 12% aqueous solution of urea, regulates pH to 8.6, sprays conical flask with dry ice subsequently
Surface 50s, centrifugation, remove supernatant, collects three times and separate lower sediment things, by it and once and secondary separation precipitate
Merge;Above-mentioned gained sediment separate out is proceeded in tube type resistance furnace, in resistance furnace, is passed through nitrogen with 3mL/min speed and protects
Protect, be subsequently heated and be warming up to 160 DEG C, heat treated 30min, under nitrogen guard mode, cool to room temperature with the furnace, obtain tea soap
Element.
The concrete application process of the present invention: weigh 5g gained of the present invention tea saponin, be dissolved in 120mL deionized water, configuration
Become solution, subsequently solution is heated to 55 DEG C, put into 15g raw wool, immersion treatment 5min, per minute stir once, with
Same mode is washed 5 times, is finally squeezed gently by solution and goes, proceeds to, in 105 DEG C of baking ovens, be dried to constant weight, subsequently will be dry with filter paper
Pilus Caprae seu Ovis after dry is spooled, and puts in apparatus,Soxhlet's, adds 120mL ether, under the conditions of 75 DEG C, and extraction 30min, discharging, will
Pilus Caprae seu Ovis proceeds in 105 DEG C of baking ovens, is dried to constant weight, and the Pilus Caprae seu Ovis color and luster after process is pure white, and feel is fluffy soft and smooth, after testing, and residual
Oils and fats rate is only 0.5%, and more conventional Wool detergent improves more than 50%.
Example 2
Weigh 260g camellia seed meal, be placed on stone grinder mill and pulverize, collect 90 mesh camellia seed meal powder, proceed to fill
In the Soxhlet extractor of 2L ethyl acetate, under the conditions of 77 DEG C, extracting 1.5h, sucking filtration removes filtrate, and gained filter cake is placed in 63
In DEG C baking oven, dried 3h, obtain defat camellia seed meal powder;Weigh 40g above-mentioned gained defat camellia seed meal powder, add and contain
Have in the beaker of 180mL deionized water, add 3g cellulase and 3g pectase, subsequently beaker is placed in digital display and tests the speed constant temperature
On magnetic stirring apparatus, it is heated to 48 DEG C, regulation rotating speed to 360r/min, after stirring reaction 40min, it is heated to 82
DEG C, add 260mL mass concentration 75% ethanol solution, then beaker proceeded in sonic oscillation instrument, regulation supersonic frequency to 30kHz,
Oscillation treatment 15min, proceeds to centrifuge, centrifugation by the mixed liquor in beaker, takes supernatant;In conical flask, add
70mL above-mentioned gained supernatant, dropping mass concentration is 13% aqueous solution of urea, and regulation pH value of solution, to 8.1, sprays with liquid nitrogen subsequently
Conical flask surface 25s, centrifugation, collect first separation lower sediment thing, proceeded in beaker, and collect supernatant, turn
Entering in conical flask, continuing dropping mass concentration is 13% aqueous solution of urea, regulates pH to 8.4, sprays conical flask table with dry ice subsequently
Face 40s, centrifugation, collect secondary separation lower sediment thing, it is merged with first separation precipitate, and collects supernatant,
Proceeding in conical flask, continuing dropping mass concentration is 13% aqueous solution of urea, regulates pH to 8.7, sprays conical flask with dry ice subsequently
Surface 55s, centrifugation, remove supernatant, collects three times and separate lower sediment things, by it and once and secondary separation precipitate
Merge;Above-mentioned gained sediment separate out is proceeded in tube type resistance furnace, in resistance furnace, is passed through nitrogen with 4mL/min speed and protects
Protect, be subsequently heated and be warming up to 170 DEG C, heat treated 35min, under nitrogen guard mode, cool to room temperature with the furnace, obtain tea soap
Element.
The concrete application process of the present invention: weigh 4g gained of the present invention tea saponin, be dissolved in 110mL deionized water, configuration
Become solution, subsequently solution is heated to 52 DEG C, put into 12g raw wool, immersion treatment 4min, per minute stir once, with
Same mode is washed 4 times, is finally squeezed gently by solution and goes, proceeds to, in 100 DEG C of baking ovens, be dried to constant weight, subsequently will be dry with filter paper
Pilus Caprae seu Ovis after dry is spooled, and puts in apparatus,Soxhlet's, adds 110mL ether, under the conditions of 72 DEG C, and extraction 25min, discharging, will
Pilus Caprae seu Ovis proceeds in 100 DEG C of baking ovens, is dried to constant weight, and the Pilus Caprae seu Ovis color and luster after process is pure white, and feel is fluffy soft and smooth, after testing, and residual
Oils and fats rate is only 0.3%, and more conventional Wool detergent improves more than 50%.
Example 3
Weigh 300g camellia seed meal, be placed on stone grinder mill and pulverize, collect 100 mesh camellia seed meal powder, proceed to contain
Having in the Soxhlet extractor of 1~3L ethyl acetate, under the conditions of 80 DEG C, extract 2h, sucking filtration removes filtrate, is placed in by gained filter cake
In 65 DEG C of baking ovens, dried 4h, obtain defat camellia seed meal powder;Weigh 50g above-mentioned gained defat camellia seed meal powder, add
Fill in the beaker of 200mL deionized water, add 4g cellulase and 4g pectase, subsequently beaker is placed in digital display and tests the speed perseverance
On temperature magnetic stirring apparatus, it is heated to 50 DEG C, regulation rotating speed to 400r/min, after stirring reaction 50min, it is heated to 85
DEG C, adding 300mL mass concentration is 80% ethanol solution, then is proceeded to by beaker in sonic oscillation instrument, and regulation supersonic frequency is extremely
35kHz, oscillation treatment 20min, the mixed liquor in beaker is proceeded to centrifuge, centrifugation, takes supernatant;In conical flask,
Adding 80mL above-mentioned gained supernatant, dropping mass concentration is 15% aqueous solution of urea, and regulation pH value of solution, to 8.2, uses liquid nitrogen subsequently
Spray conical flask surface 30s, centrifugation, collect first separation lower sediment thing, proceeded in beaker, and collect supernatant
Liquid, proceeds in conical flask, and continuing dropping mass concentration is 15% aqueous solution of urea, regulates pH to 8.5, sprays cone with dry ice subsequently
Shape bottle surface 45s, centrifugation, collect secondary separation lower sediment thing, it is merged with first separation precipitate, and collect
Clear liquid, proceeds in conical flask, and continuing dropping mass concentration is 15% aqueous solution of urea, regulates pH to 8.8, sprays with dry ice subsequently
Conical flask surface 60s, centrifugation, remove supernatant, collects three times and separate lower sediment things, by it and once and secondary separation
Precipitate merges;Above-mentioned gained sediment separate out is proceeded in tube type resistance furnace, in resistance furnace, is passed through nitrogen with 5mL/min speed
Gas shielded, is subsequently heated and is warming up to 180 DEG C, and heat treated 40min under nitrogen guard mode, cools to room temperature with the furnace, to obtain final product
Tea saponin.
The concrete application process of the present invention: weigh 3g gained of the present invention tea saponin, be dissolved in 100mL deionized water, configuration
Become solution, subsequently solution is heated to 50 DEG C, put into 10g raw wool, immersion treatment 3min, per minute stir once, with
Same mode is washed 3 times, is finally squeezed gently by solution and goes, proceed to, in 95 DEG C of baking ovens, be dried to constant weight, will be dried with filter paper subsequently
After Pilus Caprae seu Ovis spool, put in apparatus,Soxhlet's, add 100mL ether, under the conditions of 70 DEG C, extract 20min, discharging, by sheep
Hair proceeds in 95 DEG C of baking ovens, is dried to constant weight, and the Pilus Caprae seu Ovis color and luster after process is pure white, and feel is fluffy soft and smooth, after testing, remains oils and fats
Rate is only 0.2%, and more conventional Wool detergent improves more than 50%.