CN103497987A - 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 turmeric saponin clean preparation method.Background technology
Yellow ginger formal name used at school Rhizome of Peltate Yam (Dioscorea zingiberensis.C.H.Wright), have another name called the duration and degree of heating root, with root stock, is used as medicine, and is China's tradition parts of generic medicinal plants, and the title of " medicinal gold " is arranged.Contain abundant dioscin in the yellow ginger root stock, its hydrolysate is that diosgenin is turmeric saponin, and the plant that saponin content is higher in the world is few, mainly is distributed in China and Mexico.At present, the saponin export volume of China is only second to Mexico, occupies the second in the world.
At present industrial mainly by yellow ginger for the production of saponin, but the turmeric saponin extraction process has produced a large amount of waste water, polluted environment, when being dioscin is converted into to saponin, subject matter carries out acid hydrolysis, produce a large amount of acid waste water, waste water is difficult, and the resources such as the Mierocrystalline cellulose in saponin, starch could not well be utilized simultaneously, cause waste water BOD and COD very high.
Summary of the invention
The object of the present invention is to provide a kind of turmeric saponin clean preparation method, high-efficiency environment friendly, just can extract saponin without acid hydrolysis, realizes separating cellulosic in saponin and starch simultaneously.
The present invention is achieved through the following technical solutions:
A kind of turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension;
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 4-6%, in every 100ml mixed solution, add in proportion 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 and 0.4-0.6g casein hydrolysate to obtain fermention medium, 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 is cooling, carrying out bio-transformation at 34-38 ℃ of bottom fermentation cultivation 2-3d is saponin by dioscin;
3) the pH value of the fermented liquid that obtains 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 to 50-60 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue;
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin.
Further, in step 1), adopt 80-100 purpose filter cloth to be filtered, be divided into three layers after leaching the standing 5-6h of thing.
Rotating speed when further, step 2), suspension is centrifugal is 3000-4000r/min, and centrifugation time is 10-15min; Temperature during sterilizing is 121 ℃, sterilization time 20-30min.
Further, regulate the pH value of fermented liquid in step 3) after fermentation ends with the NaOH solution of 0.75-1.25mol/L.
Further, the rotating speed in step 3) during the fermented liquid centrifugation is 5000-7000r/min, and centrifugation time is 10-15min.
Further, while in step 3), the fermented liquid precipitation being extracted, add precipitation capacity 2-4 extraction using alcohol 3-4h doubly to complete the saponin extraction.
Further, the nanofiltration membrane that is 700Dalton by the fermented liquid clear liquid through molecular weight cut-off in step 3) is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
Further, repeatedly extract suction filtration liquid at least 3 times with the sherwood oil of taking out filtrate volume 1/3-1/2 in step 4).
Further again, it also comprises that processing comprises the steps: to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue by obtaining in step 1) and washing
A. in fibrous residue, add massfraction to be respectively the wheat bran of 15-25%, the ammonium sulfate of 0.5-1.5% and the tween 80 that the volume mass mark is 0.08-0.12%, and stir, then sterilizing is cooled to the 30-40 ℃ of inoculum size access viride that by volume massfraction is 8-12% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina;
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 8-12g in every liter of enzymolysis solution
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 sal epsom of 0.2-0.4g, the manganous sulfate of 0.05-0.08g and the dipotassium hydrogen phosphate of 3.0-5.0g, stir and regulate the pH value and obtain the enzymolysis nutrient solution to 5.5-6.5, access in proportion 3-5ml Paula enlightening yeast and 5-7ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud;
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Further, the temperature in step a during sterilizing is 121 ℃, sterilization time 20-30min; Temperature during constant temperature culture is 27-33 ℃, and the time is 3-5d; Temperature in step b during sterilizing is 121 ℃, sterilization time 20-25min; Temperature during fermentation is 33-39 ℃, and fermentation time is 48-60h.
Compared with prior art, the present invention has following useful technique effect:
A kind of turmeric saponin clean preparation method of the present invention, first by the starch in yellow ginger, fibrous residue and dioscin separately, hold back dioscin by nanofiltration again, utilizing the Lactobacterium acidophilum bio-transformation is saponin by the bio-transformation of 70-80% dioscin, and unconverted dioscin can be received to the recovery of nanofiltration again again for the bio-transformation of production of saponin next time, avoided acid hydrolysis in the technique of whole extraction saponin, wastewater treatment is simple, residue after suction filtration can be used as fertilizer, whole pollution is little, clean and safe, environmentally friendly; Significantly improved the transformation efficiency of dioscin in the yellow ginger, by separating of starch and fibrous residue, also avoided waste water BOD and the too high problem of COD simultaneously.
Further, by the extraction and application to cellulosic in yellow ginger and starch, by starch after liquefying-saccharifying for cultivating probiotic bacterium, the yellow ginger fibrous residue is for the production of cellulase, can obtain tropina, then the yellow ginger slag of probiotic bacterium and cellulase tropina is mixed with and obtains the yellow ginger activated feed simultaneously; Utilized efficiently the yellow ginger resource, the pollution of having avoided waste to bring; When obtaining saponin, also obtained being rich in the yellow ginger activated feed of Paula enlightening yeast, Lactobacterium acidophilum, viride and cellulase, it not only can 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 turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension; Concrete, adopt 100 purpose filter clothes to be filtered, be divided into three layers after leaching the standing 6h of thing.
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 6%, in every 100ml mixed solution, add in proportion 8ml puncture vine extracting solution, 0.3g sodium acetate, 0.5g diammonium hydrogen citrate and 0.012ml tween 80 and 0.6g casein hydrolysate to obtain fermention medium, the pH value of fermention medium is adjusted to 6.0, press 8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing is cooling, carrying out bio-transformation at 37 ℃ of bottom fermentations cultivation 3d is saponin by dioscin; Rotating speed when concrete suspension is centrifugal is 4000r/min, and centrifugation time is 15min; Temperature during sterilizing is 121 ℃, sterilization time 20min.
3) the pH value of the fermented liquid that obtains after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in to 60 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid after concrete fermentation ends with the NaOH solution of 1mol/L; Rotating speed during the fermented liquid centrifugation is 6000r/min, and centrifugation time is 15min; When the fermented liquid precipitation is extracted, add the extraction using alcohol 4h of 3 times of precipitation capacities to complete the saponin extraction; The nanofiltration membrane that is 700Dalton through molecular weight cut-off by the fermented liquid clear liquid is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin; Concrete, repeatedly extract suction filtration liquid 3 times with the sherwood oil of taking out filtrate volume 1/2.
Preferably, can be to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains in step 1) and washing, processing comprises the steps:
A. in fibrous residue, add massfraction to be respectively the tween 80 that 20% wheat bran, 1.0% ammonium sulfate and volume mass mark are 0.08%, i.e. the mass ratio of the volume of tween 80 and fibrous residue, and stir; Then sterilizing is cooled to 35 ℃ of inoculum size access viride, i.e. volumes of viride liquid spawn and the ratio of the cooling rear fibrous residue of sterilizing with the mixed total mass of admixture that by volume massfraction is 10% again; After constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 ℃, sterilization time 20min; Temperature during constant temperature culture is 30 ℃, and the time is 3d.
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 10g in every liter of enzymolysis solution
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 sal epsom of 0.3g, the manganous sulfate of 0.06g and the dipotassium hydrogen phosphate of 4.0g, stir and regulate pH value to 6.0 after obtain the enzymolysis nutrient solution, access in proportion 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud; Concrete, temperature during sterilizing is 121 ℃, sterilization time 20min; Temperature during fermentation is 37 ℃, and fermentation time is 60h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Example 2
A kind of turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension; Concrete, adopt 80 purpose filter clothes to be filtered, be divided into three layers after leaching the standing 5h of thing.
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 5%, in every 100ml mixed solution, add in proportion 6ml puncture vine extracting solution, 0.2g sodium acetate, 0.4g diammonium hydrogen citrate and 0.01ml tween 80 and 0.4g casein hydrolysate to obtain fermention medium, the pH value of fermention medium is adjusted to 5.5, press 7% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing is cooling, carrying out bio-transformation at 37 ℃ of bottom fermentations cultivation 2.5d is saponin by dioscin; Rotating speed when concrete suspension is centrifugal is 3000r/min, and centrifugation time is 10min; Temperature during sterilizing is 121 ℃, sterilization time 20min.
3) the pH value of the fermented liquid that obtains after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in to 60 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid after concrete fermentation ends with the NaOH solution of 1mol/L; Rotating speed during the fermented liquid centrifugation is 6000r/min, and centrifugation time is 14min; When the fermented liquid precipitation is extracted, add the extraction using alcohol 3.5h of 3 times of precipitation capacities to complete the saponin extraction; The nanofiltration membrane that is 700Dalton through molecular weight cut-off by the fermented liquid clear liquid is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin; Concrete, repeatedly extract suction filtration liquid 3 times with the sherwood oil of taking out filtrate volume 1/2.
Preferably, can be to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains in step 1) and washing, processing comprises the steps:
A. in fibrous residue, add massfraction to be respectively the tween 80 that 20% wheat bran, 1.0% ammonium sulfate and volume mass mark are 0.08%, and stir, then sterilizing is cooled to 35 ℃ of inoculum size access virides that by volume massfraction is 10% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 ℃, sterilization time 20min; Temperature during constant temperature culture is 30 ℃, and the time is 3d.
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 10g in every liter of enzymolysis solution
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 sal epsom of 0.3g, the manganous sulfate of 0.06g and the dipotassium hydrogen phosphate of 4.0g, stir and regulate pH value to 6.0 after obtain the enzymolysis nutrient solution, access in proportion 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud; Concrete, temperature during sterilizing is 121 ℃, sterilization time 20min; Temperature during fermentation is 37 ℃, and fermentation time is 60h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Example 3
A kind of turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension; Concrete, adopt 85 purpose filter clothes to be filtered, be divided into three layers after leaching the standing 5h of thing.
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 4%, in every 100ml mixed solution, add in proportion 7ml puncture vine extracting solution, 0.3g sodium acetate, 0.3g diammonium hydrogen citrate and 0.008ml tween 80 and 0.5g casein hydrolysate to obtain fermention medium, the pH value of fermention medium is adjusted to 5.0, press 5% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing is cooling, carrying out bio-transformation at 34 ℃ of bottom fermentations cultivation 2d is saponin by dioscin; Rotating speed when concrete suspension is centrifugal is 4000r/min, and centrifugation time is 14min; Temperature during sterilizing is 121 ℃, sterilization time 30min.
3) the pH value of the fermented liquid that obtains after fermentation ends is adjusted to 6.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in to 50 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid after concrete fermentation ends with the NaOH solution of 0.75mol/L; Rotating speed during the fermented liquid centrifugation is 5000r/min, and centrifugation time is 10min; When the fermented liquid precipitation is extracted, add the extraction using alcohol 3h of 2 times of precipitation capacities to complete the saponin extraction; The nanofiltration membrane that is 700Dalton through molecular weight cut-off by the fermented liquid clear liquid is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin; Concrete, repeatedly extract suction filtration liquid 4 times with the sherwood oil of taking out filtrate volume 1/3.
Preferably, can be to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains in step 1) and washing, processing comprises the steps:
A. in fibrous residue, add massfraction to be respectively the tween 80 that 15% wheat bran, 0.5% ammonium sulfate and volume mass mark are 0.12%, and stir, then sterilizing is cooled to 30 ℃ of inoculum size access virides that by volume massfraction is 8% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 ℃, sterilization time 30min; Temperature during constant temperature culture is 27 ℃, and the time is 4d.
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 8g in every liter of enzymolysis solution
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 sal epsom of 0.2g, the manganous sulfate of 0.05g and the dipotassium hydrogen phosphate of 3.0g, stir and regulate pH value to 5.5 after obtain the enzymolysis nutrient solution, access in proportion 3ml Paula enlightening yeast and 5ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud; Concrete, temperature during sterilizing is 121 ℃, sterilization time 25min; Temperature during fermentation is 33 ℃, and fermentation time is 48h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Example 4
A kind of turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension; Concrete, adopt 90 purpose filter clothes to be filtered, be divided into three layers after leaching the standing 5.5h of thing.
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 6%, in every 100ml mixed solution, add in proportion 6ml puncture vine extracting solution, 0.2g sodium acetate, 0.4g diammonium hydrogen citrate and 0.009ml tween 80 and 0.4g casein hydrolysate to obtain fermention medium, the pH value of fermention medium is adjusted to 5.2, press 6% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing is cooling, carrying out bio-transformation at 38 ℃ of bottom fermentations cultivation 3d is saponin by dioscin; Rotating speed when concrete suspension is centrifugal is 3000r/min, and centrifugation time is 13min; Temperature during sterilizing is 121 ℃, sterilization time 23min.
3) the pH value of the fermented liquid that obtains after fermentation ends is adjusted to 7.5, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in to 55 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid after concrete fermentation ends with the NaOH solution of 1.25mol/L; Rotating speed during the fermented liquid centrifugation is 7000r/min, and centrifugation time is 11min; When the fermented liquid precipitation is extracted, add the extraction using alcohol 4h of 4 times of precipitation capacities to complete the saponin extraction; The nanofiltration membrane that is 700Dalton through molecular weight cut-off by the fermented liquid clear liquid is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin; Concrete, repeatedly extract suction filtration liquid 5 times with the sherwood oil of taking out filtrate volume 1/2.
Preferably, can be to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains in step 1) and washing, processing comprises the steps:
A. in fibrous residue, add massfraction to be respectively the tween 80 that 18% wheat bran, 1.5% ammonium sulfate and volume mass mark are 0.10%, and stir, then sterilizing is cooled to 35 ℃ of inoculum size access virides that by volume massfraction is 12% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 ℃, sterilization time 25min; Temperature during constant temperature culture is 33 ℃, and the time is 5d.
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 12g in every liter of enzymolysis solution
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 sal epsom of 0.4g, the manganous sulfate of 0.08g and the dipotassium hydrogen phosphate of 5.0g, stir and regulate pH value to 6.5 after obtain the enzymolysis nutrient solution, access in proportion 5ml Paula enlightening yeast and 7ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud; Concrete, temperature during sterilizing is 121 ℃, sterilization time 22min; Temperature during fermentation is 39 ℃, and fermentation time is 53h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Example 5
A kind of turmeric saponin clean preparation method, comprise the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension; Concrete, adopt 95 purpose filter clothes to be filtered, be divided into three layers after leaching the standing 6h of thing.
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 5%, in every 100ml mixed solution, add in proportion 8ml puncture vine extracting solution, 0.3g sodium acetate, 0.5g diammonium hydrogen citrate and 0.011ml tween 80 and 0.6g casein hydrolysate to obtain fermention medium, the pH value of fermention medium is adjusted to 5.7, press 8% inoculum size access Lactobacterium acidophilum of fermention medium volume after sterilizing is cooling, carrying out bio-transformation at 35 ℃ of bottom fermentations cultivation 2d is saponin by dioscin; Rotating speed when concrete suspension is centrifugal is 3500r/min, and centrifugation time is 11min; Temperature during sterilizing is 121 ℃, sterilization time 27min.
3) the pH value of the fermented liquid that obtains after fermentation ends is adjusted to 7.0, then centrifugation obtains fermented liquid clear liquid and fermented liquid precipitation; Fermented liquid is deposited in to 50 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue; Regulate the pH value of fermented liquid after concrete fermentation ends with the NaOH solution of 1mol/L; Rotating speed during the fermented liquid centrifugation is 5000r/min, and centrifugation time is 13min; When the fermented liquid precipitation is extracted, add the extraction using alcohol 3h of 3 times of precipitation capacities to complete the saponin extraction; The nanofiltration membrane that is 700Dalton through molecular weight cut-off by the fermented liquid clear liquid is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaims and retains liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin; Concrete, repeatedly extract suction filtration liquid 6 times with the sherwood oil of taking out filtrate volume 1/3.
Preferably, can be to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue that obtains in step 1) and washing, processing comprises the steps:
A. in fibrous residue, add massfraction to be respectively the tween 80 that 25% wheat bran, 1.0% ammonium sulfate and volume mass mark are 0.11%, and stir, then sterilizing is cooled to 40 ℃ of inoculum size access virides that by volume massfraction is 11% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina; Concrete, temperature during sterilizing is 121 ℃, sterilization time 30min; Temperature during constant temperature culture is 28 ℃, and the time is 5d.
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 9g in every liter of enzymolysis solution
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 sal epsom of 0.3g, the manganous sulfate of 0.07g and the dipotassium hydrogen phosphate of 4.0g, stir and regulate pH value to 6.0 after obtain the enzymolysis nutrient solution, access in proportion 4ml Paula enlightening yeast and 6ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud; Concrete, temperature during sterilizing is 121 ℃, sterilization time 23min; Temperature during fermentation is 35 ℃, and fermentation time is 57h.
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
Claims (10)
1. a turmeric saponin clean preparation method, is characterized in that, comprises the steps:
1) yellow ginger is pulverized, then filtered and obtain fibrous residue and leach thing; To leach that thing is standing is divided into three layers, upper strata is supernatant liquor, and middle level is suspension liquid, and lower floor is starch; Pour out supernatant liquor standby; Isolate lower floor's starch washing, the washing lotion after starch washing is incorporated in suspension liquid and obtains suspension;
2) obtain suspension precipitation and suspension clear liquid after suspension is centrifugal, the nanofiltration membrane that is 700Dalton with molecular weight cut-off by the suspension clear liquid is carried out the reservation liquid that membrane sepn obtains containing dioscin; To retain liquid mixes with the suspension precipitation, and adjustment obtains the mixed solution that solid content is 4-6%, in every 100ml mixed solution, add in proportion 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 and 0.4-0.6g casein hydrolysate to obtain fermention medium, 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 is cooling, carrying out bio-transformation at 34-38 ℃ of bottom fermentation cultivation 2-3d is saponin by dioscin;
3) the pH value of the fermented liquid that obtains 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 to 50-60 ℃ of oven dry, add ethanol to be extracted saponin after suction filtration obtain suction filtration liquid and residue;
4) repeatedly extract suction filtration liquid with sherwood oil, stratification, merge petroleum ether layer, after the reconcentration crystallization, obtains turmeric saponin.
2. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, in step 1), adopts 80-100 purpose filter cloth to be filtered, and is divided into three layers after leaching the standing 5-6h of thing.
3. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that step 2) in the rotating speed of suspension when centrifugal be 3000-4000r/min, centrifugation time is 10-15min; Temperature during sterilizing is 121 ℃, sterilization time 20-30min.
4. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, regulates the pH value of fermented liquid in step 3) after fermentation ends with the NaOH solution of 0.75-1.25mol/L.
5. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, the rotating speed in step 3) during the fermented liquid centrifugation is 5000-7000r/min, and centrifugation time is 10-15min.
6. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, while in step 3), the fermented liquid precipitation being extracted, adds precipitation capacity 2-4 extraction using alcohol 3-4h doubly to complete the saponin extraction.
7. a kind of turmeric saponin clean preparation method according to claim 1, it is characterized in that, the nanofiltration membrane that is 700Dalton by the fermented liquid clear liquid through molecular weight cut-off in step 3) is carried out membrane sepn and is obtained the reservation liquid containing unconverted dioscin, reclaim to retain liquid when turmeric saponin is produced next time, step 2) in bio-transformation.
8. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, in step 4), with the sherwood oil of taking out filtrate volume 1/3-1/2, repeatedly extracts suction filtration liquid at least 3 times.
9. a kind of turmeric saponin clean preparation method according to claim 1, is characterized in that, also comprises that processing comprises the steps: to the processing treatment of the Dioscorea. zingiberensis Wright Starch after the fibrous residue by obtaining in step 1) and washing
A. in fibrous residue, add massfraction to be respectively the wheat bran of 15-25%, the ammonium sulfate of 0.5-1.5% and the tween 80 that the volume mass mark is 0.08-0.12%, and stir, then sterilizing is cooled to the 30-40 ℃ of inoculum size access viride that by volume massfraction is 8-12% again, after constant temperature culture, obtain the yellow ginger fibrous residue of cellulase and tropina;
B. Dioscorea. zingiberensis Wright Starch is sized mixing with the supernatant liquor obtained in step 1), obtained the enzymolysis solution of Dioscorea. zingiberensis Wright Starch through liquefaction, saccharification, by after the enzymolysis solution cooling, added in proportion (the NH of 8-12g in every liter of enzymolysis solution
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 sal epsom of 0.2-0.4g, the manganous sulfate of 0.05-0.08g and the dipotassium hydrogen phosphate of 3.0-5.0g, stir and regulate the pH value and obtain the enzymolysis nutrient solution to 5.5-6.5, access in proportion 3-5ml Paula enlightening yeast and 5-7ml Lactobacterium acidophilum after sterilizing is cooling in every 100ml enzymolysis nutrient solution, after fermentation, by solid-liquid separation, obtain probiotics bacterial mud;
C. probiotics bacterial mud is added in the yellow ginger fibrous residue of cellulase and tropina, mix also and obtain the yellow ginger activated feed after oven drying at low temperature.
10. a kind of turmeric saponin clean preparation method according to claim 9, is characterized in that, the temperature in step a during sterilizing is 121 ℃, sterilization time 20-30min; Temperature during constant temperature culture is 27-33 ℃, and the time is 3-5d; Temperature in step b during sterilizing is 121 ℃, sterilization time 20-25min; Temperature during fermentation is 33-39 ℃, and fermentation time is 48-60h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541959A (en) * | 2016-01-22 | 2016-05-04 | 竹山县鑫源皂素有限责任公司 | Extraction method of turmeric saponin |
| 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 |
| CN106831933A (en) * | 2017-01-22 | 2017-06-13 | 嵊州市派特普科技开发有限公司 | The method that thick Total saponin is extracted from Chinese yam class plant |
| CN108095187A (en) * | 2017-11-24 | 2018-06-01 | 云南中烟工业有限责任公司 | A kind of enrichment method of tobacco glucosides |
| CN108220191A (en) * | 2017-12-30 | 2018-06-29 | 陕西科技大学 | A kind of probiotics and preparation method and application |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1673385A (en) * | 2004-03-25 | 2005-09-28 | 刘华祥 | Method for producing citrin and saponin from tuber crops by biotechnology |
| CN101633686A (en) * | 2009-09-01 | 2010-01-27 | 崔黔成 | Diosgenin production process for utilizing waste water and residue as resources |
| CN103146795A (en) * | 2012-12-27 | 2013-06-12 | 西安绿泉生物技术有限公司 | Method for producing diosgenin through microbial fermentation of peltate yam rhizome-yellow ginger |
-
2013
- 2013-09-16 CN CN201310422041.5A patent/CN103497987B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1673385A (en) * | 2004-03-25 | 2005-09-28 | 刘华祥 | Method for producing citrin and saponin from tuber crops by biotechnology |
| CN101633686A (en) * | 2009-09-01 | 2010-01-27 | 崔黔成 | Diosgenin production process for utilizing waste water and residue as resources |
| CN103146795A (en) * | 2012-12-27 | 2013-06-12 | 西安绿泉生物技术有限公司 | Method for producing diosgenin through microbial fermentation of peltate yam rhizome-yellow ginger |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541959A (en) * | 2016-01-22 | 2016-05-04 | 竹山县鑫源皂素有限责任公司 | Extraction method of turmeric saponin |
| 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 |
| CN106831933A (en) * | 2017-01-22 | 2017-06-13 | 嵊州市派特普科技开发有限公司 | The method that thick Total saponin is extracted from Chinese yam class plant |
| CN108095187A (en) * | 2017-11-24 | 2018-06-01 | 云南中烟工业有限责任公司 | A kind of enrichment method of tobacco glucosides |
| CN108220191A (en) * | 2017-12-30 | 2018-06-29 | 陕西科技大学 | A kind of probiotics and preparation method and application |
| CN114934092A (en) * | 2022-06-07 | 2022-08-23 | 陕西科技大学 | Method for preparing diosgenin by biotransformation |
| CN114934092B (en) * | 2022-06-07 | 2023-08-11 | 陕西科技大学 | Method for preparing dioscin by biotransformation |
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