The content of the invention
Present invention mainly solves technical problem:Occur for traditional Tea Saponin in extraction process, water seaoning extraction
When Tea Saponin yield and purity it is low, limit the application of Tea Saponin, and when organic solvent extracts, methanol used is poisonous,
Though being increased with ethanol DNA purity compared with water extraction, the problem of high-purity is unable to reach, there is provided one kind is from camellia seed meal
The method for extracting Tea Saponin, the present invention is using camellia seed meal as raw material, after crushed, degreasing is extracted with ethyl acetate, then with enzyme
Reason, makes its intracellular active ingredient fully discharge, and then coordinates ultrasonic extraction with ethanol, recycles urea to coordinate dry ice cooling,
Recrystallization, precipitates Tea Saponin, finally heats sediment, residual ethanol is volatilized, and urea decomposes, and finally gives high-purity tea
Saponin solid.Gained Tea Saponin organic solvent-free of the invention remains, and can completely decompose, be taken out of by nitrogen stream, institute after Urea
Tea Saponin purity is obtained up to more than 98%.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)200~300g camellia seed meals are weighed, is placed on stone mill mill and pulverizes, collect 80~100 mesh oil teas
Seed dregs of rice powder, it is transferred in the Soxhlet extractor for filling 1~3L ethyl acetate, under the conditions of 75~80 DEG C, extracts 1~2h, filter
Filtrate is removed, gained filter cake is placed in 60~65 DEG C of baking ovens, 2~4h of drying process, obtains degreasing camellia seed meal powder;
(2)The above-mentioned gained degreasing camellia seed meal powder of 30~50g is weighed, adds the burning for filling 100~200mL deionized waters
In cup, 2~4g cellulases and 2~4g pectases are added, beaker then is placed in into digital display tests the speed in constant temperature blender with magnetic force,
It is heated to 45~50 DEG C, regulation rotating speed to 300~400r/min, after 30~50min of stirring reaction, it is heated to 80~
85 DEG C, it is 70~80% ethanol solutions to add 200~300mL mass concentrations, then beaker is transferred in sonic oscillation instrument, and regulation is super
Mixed liquor in beaker is transferred to centrifuge, centrifuges, take by acoustic frequency to 25~35kHz, 10~20min of oscillation treatment
Clear liquid;
(3)In conical flask, the above-mentioned gained supernatants of 60~80mL are added, dropwise addition mass concentration is 12~15% urea waters
Solution, regulation pH value of solution to 8.0~8.2, taper 20~30s of bottle surface then is sprayed with liquid nitrogen, centrifuged, collection once divides
From lower sediment thing, be transferred in beaker, and collect supernatant, be transferred in conical flask, continue be added dropwise mass concentration be 12~
15% aqueous solution of urea, pH to 8.3~8.5 is adjusted, then spray taper 35~45s of bottle surface with dry ice, centrifuged, collected
Secondary separation lower sediment thing, it is merged with first separation sediment, and collect supernatant, be transferred in conical flask, continue to drip
It is 12~15% aqueous solution of urea to add mass concentration, adjusts pH to 8.6~8.8, then with dry ice spray taper bottle surface 50~
60s, centrifuge, remove supernatant, collection separates lower sediment thing, itself and primary and secondary sediment separate out are closed three times
And;
(4)Above-mentioned gained sediment separate out is transferred in tube type resistance furnace, led to 3~5mL/min speed into resistance furnace
Enter nitrogen protection, be subsequently heated and be warming up to 160~180 DEG C, heat 30~40min, it is cold with stove under nitrogen guard mode
But to room temperature, Tea Saponin is produced.
The concrete application method of the present invention:3~5g present invention gained Tea Saponins are weighed, are dissolved in 100~120mL deionized waters
In, solution is configured to, solution is then heated to 50~55 DEG C, is put into 10~15g raw wools, 3~5min of immersion treatment,
It is per minute to stir once, wash in the same way 3~5 times, finally solution is gently squeezed and gone, is transferred in 95~105 DEG C of baking ovens, is done
It is dry then dried wool to be spooled with filter paper, is put into apparatus,Soxhlet's to constant weight, 100~120mL ether is added,
Under the conditions of 70~75 DEG C, 20~30min is extracted, discharging, wool is transferred in 95~105 DEG C of baking ovens, drying to constant weight, after processing
Wool color and luster it is pure white, feel is fluffy soft and smooth, after testing, residual grease rate be only 0.2~0.5%, more conventional wool emulsifying agent carries
It is high by more than 50%.
Beneficial effects of the present invention:
(1)It is raw material that the present invention, which utilizes the camellia seed meal after oil-producing, improves the value of camellia seed meal, is increased for peasant
Add revenue source;
(2)Present invention process short flow, the recovery rate of Tea Saponin is improved, and purity improves up to more than 98%
The application of Tea Saponin, there is wide market application foreground.
Embodiment:
200~300g camellia seed meals are weighed, is placed on stone mill mill and pulverizes, collect 80~100 mesh tea seeds
Dregs of rice powder, it is transferred in the Soxhlet extractor for filling 1~3L ethyl acetate, under the conditions of 75~80 DEG C, extracts 1~2h, suction filtration removes
Filtrate is gone, gained filter cake is placed in 60~65 DEG C of baking ovens, 2~4h of drying process, obtains degreasing camellia seed meal powder;Weigh 30~
The above-mentioned gained degreasing camellia seed meal powder of 50g, add in the beaker for filling 100~200mL deionized waters, add 2~4g fibres
Plain enzyme and 2~4g pectase is tieed up, beaker then is placed in into digital display tests the speed in constant temperature blender with magnetic force, is heated to 45~50
DEG C, regulation rotating speed is to 300~400r/min, after 30~50min of stirring reaction, is heated to 80~85 DEG C, add 200~
300mL mass concentrations are 70~80% ethanol solutions, then beaker is transferred in sonic oscillation instrument, regulation supersonic frequency to 25~
35kHz, 10~20min of oscillation treatment, the mixed liquor in beaker is transferred to centrifuge, centrifuges, take supernatant;In conical flask
In, the above-mentioned gained supernatants of 60~80mL are added, dropwise addition mass concentration is 12~15% aqueous solution of urea, regulation pH value of solution to 8.0
~8.2, taper 20~30s of bottle surface then is sprayed with liquid nitrogen, is centrifuged, first separation lower sediment thing is collected, by its turn
Enter in beaker, and collect supernatant, be transferred in conical flask, it is 12~15% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH
To 8.3~8.5, taper 35~45s of bottle surface then is sprayed with dry ice, is centrifuged, collection secondary separation lower sediment thing will
It merges with first separation sediment, and collects supernatant, is transferred in conical flask, and it is 12~15% urine to continue that mass concentration is added dropwise
The plain aqueous solution, pH to 8.6~8.8 is adjusted, then spray taper 50~60s of bottle surface with dry ice, centrifuged, remove supernatant
Liquid, collection separate lower sediment thing, it are merged with primary and secondary sediment separate out three times;By above-mentioned gained sediment separate out
It is transferred in tube type resistance furnace, nitrogen protection is passed through into resistance furnace with 3~5mL/min speed, be subsequently heated and be warming up to 160~
180 DEG C, heat 30~40min, under nitrogen guard mode, cool to room temperature with the furnace, produce Tea Saponin.
Example 1
200g camellia seed meals are weighed, is placed on stone mill mill and pulverizes, 80 mesh camellia seed meal powder is collected, is transferred to
In the Soxhlet extractor for filling 1L ethyl acetate, under the conditions of 75 DEG C, 1h is extracted, filters and removes filtrate, gained filter cake is placed in
In 60 DEG C of baking ovens, drying process 2h, degreasing camellia seed meal powder is obtained;The above-mentioned gained degreasing camellia seed meal powder of 30g is weighed, is added
In the beaker for filling 100mL deionized waters, 2g cellulases and 2g pectases are added, beaker then is placed in into digital display tests the speed perseverance
On warm magnetic stirring apparatus, 45 DEG C are heated to, regulation rotating speed to 300r/min, after stirring reaction 30min, be heated to 80
DEG C, it be 70% ethanol solution to add 200mL mass concentrations, then beaker is transferred in sonic oscillation instrument, adjust supersonic frequency to
25kHz, oscillation treatment 10min, the mixed liquor in beaker is transferred to centrifuge, centrifuges, take supernatant;In conical flask,
The above-mentioned gained supernatants of 60mL are added, dropwise addition mass concentration is 12% aqueous solution of urea, and regulation pH value of solution then uses liquid nitrogen to 8.0
Taper bottle surface 20s is sprayed, is centrifuged, first separation lower sediment thing is collected, is transferred in beaker, and collect supernatant
Liquid, it is transferred in conical flask, it is 12% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.3, is then sprayed and bored with dry ice
Shape bottle surface 35s, centrifuge, collect secondary separation lower sediment thing, it is merged with first separation sediment, and collect
Clear liquid, it is transferred in conical flask, it is 12% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.6, is then sprayed with dry ice
Taper bottle surface 50s, centrifuge, remove supernatant, collection separates lower sediment thing, it is separated with primary and secondary three times
Sediment merges;Above-mentioned gained sediment separate out is transferred in tube type resistance furnace, nitrogen is passed through into resistance furnace with 3mL/min speed
Gas shielded, it is subsequently heated and is warming up to 160 DEG C, heats 30min, under nitrogen guard mode, cool to room temperature with the furnace, produce
Tea Saponin.
The concrete application method of the present invention:5g present invention gained Tea Saponins are weighed, is dissolved in 120mL deionized waters, configures
Into solution, solution is then heated to 55 DEG C, is put into 15g raw wools, immersion treatment 5min is per minute to stir once, with
Same mode is washed 5 times, is finally gently squeezed solution and is gone, is transferred in 105 DEG C of baking ovens, is dried to constant weight, then will be dry with filter paper
Wool after dry is spooled, and is put into apparatus,Soxhlet's, adds 120mL ether, under the conditions of 75 DEG C, is extracted 30min, is discharged, will
Wool is transferred in 105 DEG C of baking ovens, is dried to constant weight, and the wool color and luster after processing is pure white, and feel is fluffy soft and smooth, after testing, residual
Grease rate is only 0.5%, and more conventional Wool detergent improves more than 50%.
Example 2
260g camellia seed meals are weighed, is placed on stone mill mill and pulverizes, 90 mesh camellia seed meal powder is collected, is transferred to
In the Soxhlet extractor for filling 2L ethyl acetate, under the conditions of 77 DEG C, 1.5h is extracted, filters and removes filtrate, gained filter cake is put
In 63 DEG C of baking ovens, drying process 3h, degreasing camellia seed meal powder is obtained;The above-mentioned gained degreasing camellia seed meal powder of 40g is weighed, is added
In the beaker for entering to fill 180mL deionized waters, 3g cellulases and 3g pectases are added, beaker then is placed in into digital display tests the speed
In constant temperature blender with magnetic force, 48 DEG C are heated to, regulation rotating speed to 360r/min, after stirring reaction 40min, be heated to
82 DEG C, add the ethanol solution of 260mL mass concentrations 75%, then beaker be transferred in sonic oscillation instrument, regulation supersonic frequency to
30kHz, oscillation treatment 15min, the mixed liquor in beaker is transferred to centrifuge, centrifuges, take supernatant;In conical flask,
The above-mentioned gained supernatants of 70mL are added, dropwise addition mass concentration is 13% aqueous solution of urea, and regulation pH value of solution then uses liquid nitrogen to 8.1
Taper bottle surface 25s is sprayed, is centrifuged, first separation lower sediment thing is collected, is transferred in beaker, and collect supernatant
Liquid, it is transferred in conical flask, it is 13% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.4, is then sprayed and bored with dry ice
Shape bottle surface 40s, centrifuge, collect secondary separation lower sediment thing, it is merged with first separation sediment, and collect
Clear liquid, it is transferred in conical flask, it is 13% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.7, is then sprayed with dry ice
Taper bottle surface 55s, centrifuge, remove supernatant, collection separates lower sediment thing, it is separated with primary and secondary three times
Sediment merges;Above-mentioned gained sediment separate out is transferred in tube type resistance furnace, nitrogen is passed through into resistance furnace with 4mL/min speed
Gas shielded, it is subsequently heated and is warming up to 170 DEG C, heats 35min, under nitrogen guard mode, cool to room temperature with the furnace, produce
Tea Saponin.
The concrete application method of the present invention:4g present invention gained Tea Saponins are weighed, is dissolved in 110mL deionized waters, configures
Into solution, solution is then heated to 52 DEG C, is put into 12g raw wools, immersion treatment 4min is per minute to stir once, with
Same mode is washed 4 times, is finally gently squeezed solution and is gone, is transferred in 100 DEG C of baking ovens, is dried to constant weight, then will be dry with filter paper
Wool after dry is spooled, and is put into apparatus,Soxhlet's, adds 110mL ether, under the conditions of 72 DEG C, is extracted 25min, is discharged, will
Wool is transferred in 100 DEG C of baking ovens, is dried to constant weight, and the wool color and luster after processing is pure white, and feel is fluffy soft and smooth, after testing, residual
Grease rate is only 0.3%, and more conventional Wool detergent improves more than 50%.
Example 3
300g camellia seed meals are weighed, is placed on stone mill mill and pulverizes, collect 100 mesh camellia seed meal powder, are turned
In the Soxhlet extractor for entering to fill 1~3L ethyl acetate, under the conditions of 80 DEG C, 2h is extracted, filters and removes filtrate, by gained filter cake
It is placed in 65 DEG C of baking ovens, drying process 4h, obtains degreasing camellia seed meal powder;The above-mentioned gained degreasing camellia seed meal powder of 50g is weighed,
Add in the beaker for filling 200mL deionized waters, add 4g cellulases and 4g pectases, beaker then is placed in into digital display surveys
In fast constant temperature blender with magnetic force, 50 DEG C are heated to, regulation rotating speed to 400r/min, after stirring reaction 50min, heat temperature raising
To 85 DEG C, it be 80% ethanol solution to add 300mL mass concentrations, then beaker is transferred in sonic oscillation instrument, adjust supersonic frequency to
35kHz, oscillation treatment 20min, the mixed liquor in beaker is transferred to centrifuge, centrifuges, take supernatant;In conical flask,
The above-mentioned gained supernatants of 80mL are added, dropwise addition mass concentration is 15% aqueous solution of urea, and regulation pH value of solution then uses liquid nitrogen to 8.2
Taper bottle surface 30s is sprayed, is centrifuged, first separation lower sediment thing is collected, is transferred in beaker, and collect supernatant
Liquid, it is transferred in conical flask, it is 15% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.5, is then sprayed and bored with dry ice
Shape bottle surface 45s, centrifuge, collect secondary separation lower sediment thing, it is merged with first separation sediment, and collect
Clear liquid, it is transferred in conical flask, it is 15% aqueous solution of urea to continue that mass concentration is added dropwise, and adjusts pH to 8.8, is then sprayed with dry ice
Taper bottle surface 60s, centrifuge, remove supernatant, collection separates lower sediment thing, it is separated with primary and secondary three times
Sediment merges;Above-mentioned gained sediment separate out is transferred in tube type resistance furnace, nitrogen is passed through into resistance furnace with 5mL/min speed
Gas shielded, it is subsequently heated and is warming up to 180 DEG C, heats 40min, under nitrogen guard mode, cool to room temperature with the furnace, produce
Tea Saponin.
The concrete application method of the present invention:3g present invention gained Tea Saponins are weighed, is dissolved in 100mL deionized waters, configures
Into solution, solution is then heated to 50 DEG C, is put into 10g raw wools, immersion treatment 3min is per minute to stir once, with
Same mode washes 3 times, finally gently squeezes solution and goes, is transferred in 95 DEG C of baking ovens, dries to constant weight, then with filter paper by drying
Wool afterwards is spooled, and is put into apparatus,Soxhlet's, adds 100mL ether, under the conditions of 70 DEG C, extracts 20min, discharging, by sheep
Hair is transferred in 95 DEG C of baking ovens, is dried to constant weight, and the wool color and luster after processing is pure white, and feel is fluffy soft and smooth, after testing, remains grease
Rate is only 0.2%, and more conventional Wool detergent improves more than 50%.