CN103497987B - Clean production method of yam diosgenin - Google Patents
Clean production method of yam diosgenin Download PDFInfo
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Abstract
The invention aims at providing a clean production method of yam diosgenin. The clean production method of yam diosgenin is high-efficiency and environmentallyenvironment-friendly and can be used for extracting diosgenin without needing acid hydrolysis and meanwhile realizing the separation of fibers and starch in diosgenin. The clean production method comprises the following steps: firstly separating starch, fibrous residues and dioscin in yam, then intercepting dioscin through nanofiltration, and biologically converting 70-80% of dioscin into the diosgenin by using lactobacillus acidophilus biotransformation, and wherein recycling the unconverted diosgenin can be subjected to through nanofiltration again and can be recycled and reused for biotransformation in the next production process. The clean production method has the advantages that the acid hydrolysis is avoided in the whole diosgenin extraction process, the wastewater treatment is simple, the residues obtained after suction filtration can be used as fertilizer, and the clean production method has low pollution on the whole and is clean, safe and environmentallyenvironment-friendly; and meanwhile, the conversion rate of the diosgenin in the yam is substantially increased, the starch is separated from the fibrous residues, and the problem of excessive BOD (Biochemical Oxygen Demand) and COD (Chemical Oxygen Demand) in wastewater is also avoided by separating the starch from the fibrous residues.
Description
Technical field
The present invention relates to the production field of turmeric saponin, be specially a kind of Clean production method of yam diosgenin.Background technology
Yellow ginger formal name used at school Rhizome of Peltate Yam (Dioscorea zingiberensis.C.H.Wright), has another name called duration and degree of heating root, is used as medicine with root stock, is China's tradition parts of generic medicinal plants, has the title of " medicinal gold ".Containing abundant dioscin in yellow ginger root stock, its hydrolysate is diosgenin and turmeric saponin, and the plant that saponin content is higher is in the world few, is mainly distributed in China and Mexico.At present, the saponin export volume of China is only second to Mexico, occupies the second in the world.
Current industrial main by yellow ginger for the production of saponin, but turmeric saponin extraction process creates a large amount of waste water, pollute environment, subject matter is to carry out acid hydrolysis when dioscin being converted into saponin, produce a large amount of acid waste water, waste water is difficult, and the resource such as Mierocrystalline cellulose, starch simultaneously in saponin could not well be utilized, and causes waste water BOD and COD very high.
Summary of the invention
The object of the present invention is to provide a kind of Clean production method of yam diosgenin, high-efficiency environment friendly, just can extract saponin without the need to acid hydrolysis, realize being separated cellulosic in saponin and starch simultaneously.
The present invention is achieved through the following technical solutions:
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension;
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 4-6%, 6-8ml puncture vine extracting solution, 0.2-0.3g sodium acetate, 0.3-0.5g diammonium hydrogen citrate and 0.008-0.012ml tween 80 is added in proportion and 0.4-0.6g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.0-6.0, press the 5-8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 34-38 DEG C of bottom fermentation cultivation 2-3d is saponin;
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 6.5-7.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 50-60 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue;
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin.
Further, adopt 80-100 object filter cloth to filter in step 1), much filtrate is divided into three layers after leaving standstill 5-6h.
Further, step 2) in suspension centrifugal time rotating speed be 3000-4000r/min, centrifugation time is 10-15min; Temperature during sterilizing is 121 DEG C, sterilization time 20-30min.
Further, the pH value of fermented liquid is regulated in step 3) after fermentation ends by the NaOH solution of 0.75-1.25mol/L.
Further, the rotating speed in step 3) during fermented liquid centrifugation is 5000-7000r/min, and centrifugation time is 10-15min.
Further, when fermented liquid precipitation being extracted in step 3), add precipitation capacity 2-4 extraction using alcohol 3-4h doubly and complete saponin extraction.
Further, in step 3), fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
Further, suction filtration liquid at least 3 times are repeatedly extracted with the sherwood oil taking out filtrate volume 1/3-1/2 in step 4).
Further again, it also comprises the processing treatment of the Dioscorea. zingiberensis Wright Starch after to the fibrous residue will obtained in step 1) and washing, and process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 15-25%, the ammonium sulfate of 0.5-1.5% and volume mass mark be the tween 80 of 0.08-0.12%, and stir, then sterilizing be cooled to 30-40 DEG C more by volume massfraction be 8-12% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina;
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 8-12g in proportion
4)
2sO
4, the peptone of 3-7g, the anhydrous sodium acetate of 2.0-4.0g, the diammonium hydrogen citrate of 4-8g, the tween 80 of 0.8-1.2mL, the magnesium sulfate of 0.2-0.4g, the manganous sulfate of 0.05-0.08g and 3.0-5.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 5.5-6.5, in every 100ml enzymolysis nutrient solution, access 3-5ml Paula enlightening yeast and 5-7ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation;
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Further, the temperature in step a during sterilizing is 121 DEG C, sterilization time 20-30min; Temperature during constant temperature culture is 27-33 DEG C, and the time is 3-5d; Temperature in step b during sterilizing is 121 DEG C, sterilization time 20-25min; Temperature during fermentation is 33-39 DEG C, and fermentation time is 48-60h.
Compared with prior art, the present invention has following useful technique effect:
A kind of Clean production method of yam diosgenin of the present invention, first by the starch in yellow ginger, fibrous residue and dioscin separately, dioscin is retained again by nanofiltration, Lactobacterium acidophilum bio-transformation is utilized to be saponin by the bio-transformation of 70-80% dioscin, and unconverted dioscin can be received nanofiltration again and reclaim the bio-transformation be again used in production of saponin next time, acid hydrolysis is avoided in the technique of whole extraction saponin, wastewater treatment is simple, residue after suction filtration can be used as fertilizer, overall pollution is little, clean and safe, environmentally friendly; Significantly improve the transformation efficiency of dioscin in yellow ginger simultaneously, by being separated of starch and fibrous residue, it also avoid the problem that waste water BOD and COD is too high.
Further, by the extraction and application to cellulosic in yellow ginger and starch, starch is used for after liquefying-saccharifying cultivate probiotic bacterium, yellow ginger fibrous residue is for the production of cellulase, simultaneously can obtain tropina, then the yellow ginger slag of probiotic bacterium and cellulase tropina is mixed with obtains yellow ginger activated feed; Make use of yellow ginger resource efficiently, avoid the pollution that waste brings; While obtaining saponin, also obtain the yellow ginger activated feed being rich in Paula enlightening yeast, Lactobacterium acidophilum, viride and cellulase, it can not only be the useful animal health of livestock probiotic supplemented, cellulase in feed can also promote the absorption of nutritive substance and improve efficiency of feed utilization, the value added of product is high, and productivity effect is good.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Example 1
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension; Concrete, adopt 100 object filter clothes to filter, much filtrate is divided into three layers after leaving standstill 6h.
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 6%, 8ml puncture vine extracting solution, 0.3g sodium acetate, 0.5g diammonium hydrogen citrate and 0.012ml tween 80 is added in proportion and 0.6g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 6.0, press 8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 37 DEG C of bottom fermentations cultivation 3d is saponin; Rotating speed when concrete suspension is centrifugal is 4000r/min, and centrifugation time is 15min; Temperature during sterilizing is 121 DEG C, sterilization time 20min.
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 60 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid by the NaOH solution of 1mol/L after concrete fermentation ends; Rotating speed during fermented liquid centrifugation is 6000r/min, and centrifugation time is 15min; When extracting fermented liquid precipitation, the extraction using alcohol 4h adding precipitation capacity 3 times completes saponin extraction; Fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin; Concrete, repeatedly extract suction filtration liquid 3 times with the sherwood oil taking out filtrate volume 1/2.
Preferably, can to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue obtained in step 1) and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 20%, the ammonium sulfate of 1.0% and volume mass mark be the tween 80 of 0.08%, i.e. the volume of tween 80 and the mass ratio of fibrous residue, and stir; Then sterilizing be cooled to 35 DEG C more by volume massfraction be the inoculum size access viride of 10%, namely volume and the sterilizing of viride liquid spawn cools the ratio of fibrous residue and the mixed total mass of admixture afterwards; After constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 20min; Temperature during constant temperature culture is 30 DEG C, and the time is 3d.
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 10g in proportion
4)
2sO
4, the peptone of 5g, the anhydrous sodium acetate of 3g, the diammonium hydrogen citrate of 6g, the tween 80 of 1.0mL, the magnesium sulfate of 0.3g, the manganous sulfate of 0.06g and 4.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 6.0, in every 100ml enzymolysis nutrient solution, access 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 20min; Temperature during fermentation is 37 DEG C, and fermentation time is 60h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Example 2
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension; Concrete, adopt 80 object filter clothes to filter, much filtrate is divided into three layers after leaving standstill 5h.
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 5%, 6ml puncture vine extracting solution, 0.2g sodium acetate, 0.4g diammonium hydrogen citrate and 0.01ml tween 80 is added in proportion and 0.4g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.5, press 7% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 37 DEG C of bottom fermentations cultivation 2.5d is saponin; Rotating speed when concrete suspension is centrifugal is 3000r/min, and centrifugation time is 10min; Temperature during sterilizing is 121 DEG C, sterilization time 20min.
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 60 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid by the NaOH solution of 1mol/L after concrete fermentation ends; Rotating speed during fermented liquid centrifugation is 6000r/min, and centrifugation time is 14min; When extracting fermented liquid precipitation, the extraction using alcohol 3.5h adding precipitation capacity 3 times completes saponin extraction; Fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin; Concrete, repeatedly extract suction filtration liquid 3 times with the sherwood oil taking out filtrate volume 1/2.
Preferably, can to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue obtained in step 1) and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 20%, the ammonium sulfate of 1.0% and volume mass mark be the tween 80 of 0.08%, and stir, then sterilizing be cooled to 35 DEG C more by volume massfraction be 10% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 20min; Temperature during constant temperature culture is 30 DEG C, and the time is 3d.
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 10g in proportion
4)
2sO
4, the peptone of 5g, the anhydrous sodium acetate of 3g, the diammonium hydrogen citrate of 6g, the tween 80 of 1.0mL, the magnesium sulfate of 0.3g, the manganous sulfate of 0.06g and 4.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 6.0, in every 100ml enzymolysis nutrient solution, access 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 20min; Temperature during fermentation is 37 DEG C, and fermentation time is 60h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Example 3
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension; Concrete, adopt 85 object filter clothes to filter, much filtrate is divided into three layers after leaving standstill 5h.
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 4%, 7ml puncture vine extracting solution, 0.3g sodium acetate, 0.3g diammonium hydrogen citrate and 0.008ml tween 80 is added in proportion and 0.5g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.0, press 5% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 34 DEG C of bottom fermentations cultivation 2d is saponin; Rotating speed when concrete suspension is centrifugal is 4000r/min, and centrifugation time is 14min; Temperature during sterilizing is 121 DEG C, sterilization time 30min.
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 6.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 50 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid by the NaOH solution of 0.75mol/L after concrete fermentation ends; Rotating speed during fermented liquid centrifugation is 5000r/min, and centrifugation time is 10min; When extracting fermented liquid precipitation, the extraction using alcohol 3h adding precipitation capacity 2 times completes saponin extraction; Fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin; Concrete, repeatedly extract suction filtration liquid 4 times with the sherwood oil taking out filtrate volume 1/3.
Preferably, can to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue obtained in step 1) and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 15%, the ammonium sulfate of 0.5% and volume mass mark be the tween 80 of 0.12%, and stir, then sterilizing be cooled to 30 DEG C more by volume massfraction be 8% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 30min; Temperature during constant temperature culture is 27 DEG C, and the time is 4d.
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 8g in proportion
4)
2sO
4, the peptone of 3g, the anhydrous sodium acetate of 2g, the diammonium hydrogen citrate of 4g, the tween 80 of 0.8mL, the magnesium sulfate of 0.2g, the manganous sulfate of 0.05g and 3.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 5.5, in every 100ml enzymolysis nutrient solution, access 3ml Paula enlightening yeast and 5ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 25min; Temperature during fermentation is 33 DEG C, and fermentation time is 48h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Example 4
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension; Concrete, adopt 90 object filter clothes to filter, much filtrate is divided into three layers after leaving standstill 5.5h.
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 6%, 6ml puncture vine extracting solution, 0.2g sodium acetate, 0.4g diammonium hydrogen citrate and 0.009ml tween 80 is added in proportion and 0.4g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.2, press 6% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 38 DEG C of bottom fermentations cultivation 3d is saponin; Rotating speed when concrete suspension is centrifugal is 3000r/min, and centrifugation time is 13min; Temperature during sterilizing is 121 DEG C, sterilization time 23min.
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 7.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 55 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid by the NaOH solution of 1.25mol/L after concrete fermentation ends; Rotating speed during fermented liquid centrifugation is 7000r/min, and centrifugation time is 11min; When extracting fermented liquid precipitation, the extraction using alcohol 4h adding precipitation capacity 4 times completes saponin extraction; Fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin; Concrete, repeatedly extract suction filtration liquid 5 times with the sherwood oil taking out filtrate volume 1/2.
Preferably, can to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue obtained in step 1) and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 18%, the ammonium sulfate of 1.5% and volume mass mark be the tween 80 of 0.10%, and stir, then sterilizing be cooled to 35 DEG C more by volume massfraction be 12% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 25min; Temperature during constant temperature culture is 33 DEG C, and the time is 5d.
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 12g in proportion
4)
2sO
4, the peptone of 7g, the anhydrous sodium acetate of 4g, the diammonium hydrogen citrate of 8g, the tween 80 of 1.2mL, the magnesium sulfate of 0.4g, the manganous sulfate of 0.08g and 5.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 6.5, in every 100ml enzymolysis nutrient solution, access 5ml Paula enlightening yeast and 7ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 22min; Temperature during fermentation is 39 DEG C, and fermentation time is 53h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Example 5
A kind of Clean production method of yam diosgenin, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension; Concrete, adopt 95 object filter clothes to filter, much filtrate is divided into three layers after leaving standstill 6h.
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 5%, 8ml puncture vine extracting solution, 0.3g sodium acetate, 0.5g diammonium hydrogen citrate and 0.011ml tween 80 is added in proportion and 0.6g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.7, press 8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carrying out bio-transformation by dioscin at 35 DEG C of bottom fermentations cultivation 2d is saponin; Rotating speed when concrete suspension is centrifugal is 3500r/min, and centrifugation time is 11min; Temperature during sterilizing is 121 DEG C, sterilization time 27min.
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 50 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid by the NaOH solution of 1mol/L after concrete fermentation ends; Rotating speed during fermented liquid centrifugation is 5000r/min, and centrifugation time is 13min; When extracting fermented liquid precipitation, the extraction using alcohol 3h adding precipitation capacity 3 times completes saponin extraction; Fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaims and retain liquid when being used for that turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin; Concrete, repeatedly extract suction filtration liquid 6 times with the sherwood oil taking out filtrate volume 1/3.
Preferably, can to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue obtained in step 1) and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 25%, the ammonium sulfate of 1.0% and volume mass mark be the tween 80 of 0.11%, and stir, then sterilizing be cooled to 40 DEG C more by volume massfraction be 11% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 30min; Temperature during constant temperature culture is 28 DEG C, and the time is 5d.
B. the supernatant liquor obtained in Dioscorea. zingiberensis Wright Starch step 1) is sized mixing, through the enzymolysis solution of liquefaction, saccharification acquisition Dioscorea. zingiberensis Wright Starch, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 9g in proportion
4)
2sO
4, the peptone of 6g, the anhydrous sodium acetate of 3g, the diammonium hydrogen citrate of 5g, the tween 80 of 1.0mL, the magnesium sulfate of 0.3g, the manganous sulfate of 0.07g and 4.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 6.0, in every 100ml enzymolysis nutrient solution, access 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation; Concrete, temperature during sterilizing is 121 DEG C, sterilization time 23min; Temperature during fermentation is 35 DEG C, and fermentation time is 57h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
Claims (10)
1. a Clean production method of yam diosgenin, is characterized in that, comprises the steps:
1) yellow ginger is pulverized, then filter and obtain fibrous residue and much filtrate; Much filtrate left standstill and be divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor for subsequent use; Isolate lower floor's starch and wash, the washing lotion after starch washing being incorporated in suspension liquid and obtaining suspension;
2) obtain suspension sedimentation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane being 700Dalton by suspension clear liquid molecular weight cut-off carries out the reservation liquid that membrane sepn obtains containing dioscin; Liquid will be retained mix with suspension sedimentation, and adjustment obtains the mixed solution that solid content is 4-6%, 6-8ml puncture vine extracting solution, 0.2-0.3g sodium acetate, 0.3-0.5g diammonium hydrogen citrate and 0.008-0.012ml tween 80 is added in proportion and 0.4-0.6g casein hydrolysate obtains fermention medium in every 100ml mixed solution, the pH value of fermention medium is adjusted to 5.0-6.0, press the 5-8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing cooling, carry out bio-transformation at 34-38 DEG C of bottom fermentation cultivation 2-3d and dioscin is converted into saponin;
3) pH value of the fermented liquid obtained after fermentation ends is adjusted to 6.5-7.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in 50-60 DEG C of oven dry, add ethanol carry out extraction saponin after suction filtration obtain suction filtration liquid and residue;
4) repeatedly extract suction filtration liquid, stratification with sherwood oil, merge petroleum ether layer, after reconcentration crystallization, obtain turmeric saponin.
2. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 1) in adopt 80-100 object filter cloth to filter, much filtrate is divided into three layers after leaving standstill 5-6h.
3. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 2) in suspension centrifugal time rotating speed be 3000-4000r/min, centrifugation time is 10-15min; Temperature during sterilizing is 121 DEG C, sterilization time 20-30min.
4. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 3) in regulate the pH value of fermented liquid after fermentation ends by the NaOH solution of 0.75-1.25mol/L.
5. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 3) in fermented liquid centrifugation time rotating speed be 5000-7000r/min, centrifugation time is 10-15min.
6. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 3) in when fermented liquid precipitation is extracted, add precipitation capacity 2-4 extraction using alcohol 3-4h doubly and complete saponin extraction.
7. a kind of Clean production method of yam diosgenin according to claim 1, it is characterized in that, step 3) in fermented liquid clear liquid is carried out through the nanofiltration membrane that molecular weight cut-off is 700Dalton the reservation liquid that membrane sepn obtains containing unconverted dioscin, reclaim retain liquid be used for next time turmeric saponin produce time, step 2) in bio-transformation.
8. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, step 4) in repeatedly extract suction filtration liquid at least 3 times with the sherwood oil taking out filtrate volume 1/3-1/2.
9. a kind of Clean production method of yam diosgenin according to claim 1, is characterized in that, also comprises by step 1) in the processing treatment of Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains and washing, process comprises the steps:
A. in fibrous residue, adding massfraction, to be respectively the wheat bran of 15-25%, the ammonium sulfate of 0.5-1.5% and volume mass mark be the tween 80 of 0.08-0.12%, and stir, then sterilizing be cooled to 30-40 DEG C more by volume massfraction be 8-12% inoculum size access viride, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina;
B. by Dioscorea. zingiberensis Wright Starch step 1) in the supernatant liquor that obtains size mixing, obtain the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, after being lowered the temperature by enzymolysis solution, in often liter of enzymolysis solution, add (the NH of 8-12g in proportion
4)
2sO
4, the peptone of 3-7g, the anhydrous sodium acetate of 2.0-4.0g, the diammonium hydrogen citrate of 4-8g, the tween 80 of 0.8-1.2mL, the magnesium sulfate of 0.2-0.4g, the manganous sulfate of 0.05-0.08g and 3.0-5.0g dipotassium hydrogen phosphate, stir and obtain enzymolysis nutrient solution after adjust ph to 5.5-6.5, in every 100ml enzymolysis nutrient solution, access 3-5ml Paula enlightening yeast and 5-7ml Lactobacterium acidophilum in proportion after sterilizing cooling, after fermentation, obtain probiotics bacterial mud by solid-liquid separation;
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix and obtain yellow ginger activated feed after oven drying at low temperature.
10. a kind of Clean production method of yam diosgenin according to claim 9, is characterized in that, the temperature in step a during sterilizing is 121 DEG C, sterilization time 20-30min; Temperature during constant temperature culture is 27-33 DEG C, and the time is 3-5d; Temperature in step b during sterilizing is 121 DEG C, sterilization time 20-25min; Temperature during fermentation is 33-39 DEG C, and fermentation time is 48-60h.
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| CN106086150A (en) * | 2016-07-25 | 2016-11-09 | 陕西科技大学 | A kind of method utilizing enzyme to combine microorganism conversion production turmeric saponin |
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