CN100572553C - Method with preparing dioscin with dioscin penicillium notatum - Google Patents
Method with preparing dioscin with dioscin penicillium notatum Download PDFInfo
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- CN100572553C CN100572553C CNB2006101245158A CN200610124515A CN100572553C CN 100572553 C CN100572553 C CN 100572553C CN B2006101245158 A CNB2006101245158 A CN B2006101245158A CN 200610124515 A CN200610124515 A CN 200610124515A CN 100572553 C CN100572553 C CN 100572553C
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Abstract
The invention discloses a kind of yam saponin penicillium notatum Penicillum dioscin051016 that uses, CCTCC No:M206001 prepares the method for diosgenin, relates to the preparation of diosgenin.This production method comprises: Chinese yam pulverizes, sterilizes, admixes yam saponin penicillium notatum, times 25～28 ℃ fermentations 24～36 hours in pH4～7, with sherwood oil refluxing extraction, crystallization, drying, obtain diosgenin.The present invention compared with prior art has following advantage: 1, do not produce acid organic waste water pollutent; 2, the present invention has reduced production energy consumption and production cost in normal temperature fermentation.
Description
Technical field:
The present invention relates to the preparation of diosgenin, the method that more specifically relates to the yam saponin penicillium notatum fermentation prepares diosgenin.Diosgenin is a main raw material of producing steroid hormone.
Background technology:
Diosgenin extracts from yam, and yellow ginger is a main resource of extracting diosgenin.With diosgenin is that the synthetic drug of raw material has kind more than 200, and it is raw material with the diosgenin that the steroid hormone more than 60% is wherein arranged.
The traditional method of extracting diosgenin from the Chinese yam raw material is to adopt acid hydrolyzation.Extraction process with acid hydrolyzation can produce a large amount of acid organic waste water pollution producing region environment and river, carries out sewage disposal production cost will significantly be increased.Therefore, people attempt to substitute acid hydrolyzation with other method always, avoiding the pollution to environment, and have obtained certain progress.
The method of extracting diosgenin from yellow ginger has: a, directly acid hydrolysis; Carry out acid hydrolysis again after b, the pre-fermentation; Carry out acid hydrolysis again after c, the separation; Carry out acid hydrolysis behind d, the enzymolysis again; Carry out acid hydrolysis etc. behind e, the microbial fermentation again.
A, direct acid hydrolysis are the methods that tradition is extracted diosgenin: this method is carried out acid hydrolysis with sulfuric acid or hydrochloric acid with the Chinese yam raw material earlier, hydrolyzate is neutralized to neutrality with alkaline matter, wash with water again, after the drying, use the solvent extraction diosgenin again, because saponin main form with dioscin in plant materials combines with Mierocrystalline cellulose and is present in the cell walls, again because plant cell wall is tougher, the extraction yield that therefore direct acid-hydrolysis method extracts diosgenin is lower.
Carrying out acid hydrolysis after b, the pre-fermentation again extracts the method for diosgenin and is: earlier the Chinese yam raw material is let alone many days a couple of days to ten of spontaneous fermentation before acid hydrolysis, make the amylolysis in the material, carry out acid hydrolysis again after plant materials is loose, from vegetable material, extract diosgenin then, can make the yield of diosgenin be higher than direct acid-hydrolysis method.The most producers of China all adopt this explained hereafter diosgenin now.But because multiple microorganism participates in fermentation in the spontaneous fermentation process, fermentation condition is difficult to control, and impurity increases makes the diosgenin downgrade.In order to improve the productive rate of diosgenin, except pre-fermentation method, add enzyme liquid such as cellulase, polygalacturonase, amylase, synaptase and glucuroide and carry out enzymolysis earlier, dioscin is come out, when acid hydrolysis, can improve the productive rate of diosgenin.
C, carry out acid hydrolysis after separating again and extract the method for diosgenin and be: the Chinese yam raw material is added water mill is broken to sieve, isolate fibrous residue earlier, filtered liquid is through behind the sedimentation and drawing, use extraction using alcohol after the supernatant concentration, ether sedimentation obtains water-solubility saponin, the saponin(e starch slurry adding amylase that separation is obtained carries out enzymolysis, and the sugared slag behind the enzymolysis carries out acid hydrolysis again.
The method of carrying out acid hydrolysis extraction diosgenin behind d, the enzymolysis again is people's inventions such as Huazhong Institute of Technology Zhao book Shen, this method adopts purebred black-koji mould, use raw materials for production without spontaneous fermentation, destroyed after the various enzymes that self exist through boiling, directly use the black-koji mould inoculation fermentation, extract diosgenin through sulphuric acid hydrolysis again, its productive rate improves many than the extracting method of front.
Carry out acid hydrolysis etc. behind e, the microbial fermentation again.Northwest plant research institute and Shan two provinces defend Dong Yiyaohuagongchang, operational path is divided into three parts: the first step is isolated Mierocrystalline cellulose earlier, second step inoculation strain degradation starch generates yeast powder, and obtain sugared slag, the 3rd step sugared slag that will obtain carries out acid hydrolysis, uses No. 120 gasoline or ethanol or acetone or supercritical CO again
2Extract saponin.This method is also than the extraction yield height of traditional technology, and reduced discharged waste water.
In sum, though various process modification has improved the extraction yield of diosgenin than traditional direct employing acid hydrolyzation, and reduced the quantity discharged of sour water pollutent.But all above-mentioned technologies still need be passed through acid-hydrolyzed step bar none.Therefore, all can produce acid organic waste water pollutent inevitably, and total amount is very big, and the cost of sewage disposal is very high, directly influence saponin producers' health, even more serious is a large amount of acid organic waste water pollutents have caused serious pollution to the environment and the river in producing region.
Summary of the invention:
The object of the present invention is to provide a kind of with yam saponin penicillium notatum Penicillumdioscin 051016, CCTCC No:M206001 prepares the method for diosgenin, containing in the dioscin raw material after this method is sterilized the yam saponin penicillium notatum access fermented, gained diosgenin productive rate is more than 90%, and does not produce acid organic waste water pollutent.
For achieving the above object, with yam saponin penicillium notatum Penicillum dioscin051016, the method that CCTCC No:M206001 prepares diosgenin follows these steps to carry out.
1, cleans the Chinese yam raw material;
2, with raw material crushing to 5mm;
3, directly 100 ℃ of sterilizations 0.5～1 hour, perhaps add the ammoniacal liquor of raw material weight 0.5%, mix thoroughly, placed 1 hour for 25 ℃～28 ℃;
4,25 ℃～28 ℃ yam saponin penicillium notatum Penicillumdioscin 051016 that insert raw material weight 0.1%, CCTCC No:M206001 stirs, and under PH4～7 conditions, 25 ℃～28 ℃ fermented 24～36 hours;
5, the water that adds 4 times of weight of fermentation materials;
6, stir, filter, filter residue 60 ℃～70 ℃ dryings, is added the sherwood oil of 60 ℃～90 ℃ of boiling ranges of 3～5 times of filter residue weight again;
7,60 ℃ of refluxing extraction are 2～3 times, united extraction liquid;
8,60 ℃ of recovery sherwood oil to diosgenin crystallizations are separated out;
9, filter, get the diosgenin crystallization;
10, use 60 ℃ of dissolvings of sherwood oil of 60 ℃～90 ℃ of boiling ranges of diosgenin crystallization double weight, slowly add ethanol again to the solution muddiness, placement is spent the night, recrystallization;
11, leaching crystallization, 60 ℃ of dryings obtain the crystallization of diosgenin content more than 98%.
The present invention compared with prior art has the following advantages: 1, do not produce acid organic waste water pollutent; 2, the present invention has reduced production energy consumption and production cost in normal temperature fermentation.
Specific embodiments:
Embodiment 1:
The method for preparing diosgenin with yam saponin penicillium notatum 051016 (Penicillum dioscin 051016) CCTCCNo:M206001 follows these steps to carry out.
1, cleans the Chinese yam raw material;
2, with raw material crushing to 5mm;
3, directly 100 ℃ of sterilizations 0.5～1 hour, perhaps add the ammoniacal liquor of raw material weight 0.5%, mix thoroughly, placed 1 hour for 25 ℃～28 ℃;
4,25 ℃～28 ℃ yam saponin penicillium notatum Penicillumdioscin 051016 that insert raw material weight 0.1%, CCTCC No:M206001 stirs, and under PH4～7 conditions, 25 ℃～28 ℃ fermented 24～36 hours;
5, the water that adds 4 times of weight of fermentation materials;
6, stir, filter, filter residue 60 ℃～70 ℃ dryings, is added the sherwood oil of 60 ℃～90 ℃ of boiling ranges of 3～5 times of filter residue weight again;
7,60 ℃ of refluxing extraction are 2～3 times, united extraction liquid;
8,60 ℃ of recovery sherwood oil to diosgenin crystallizations are separated out;
9, filter, get the diosgenin crystallization;
10, use 60 ℃ of dissolvings of sherwood oil of 60 ℃～90 ℃ of boiling ranges of diosgenin crystallization double weight, slowly add ethanol again to the solution muddiness, placement is spent the night, recrystallization;
11, leaching crystallization, 60 ℃ of dryings obtain the crystallization of diosgenin content more than 98%.
Implementation column 2:
The method for preparing diosgenin with yam saponin penicillium notatum 051016 (Penicillum dioscin 051016) CCTCCNo:M206001 follows these steps to carry out.
1, get 100 kilograms of Chinese yam raw materials, clean to not having silt and other impurity, through efficient liquid phase chromatographic analysis, this Chinese yam raw material contains diosgenin 2.3%;
2, the water that adds 500 kilograms is with below the Chinese yam raw material crushing to 5 millimeter;
3, will be broken material pack in the fermentor tank, add the ammoniacal liquor of 500 grams, mix 26 ℃ of airtight placements 1 hour thoroughly;
4,25 ℃ of yam saponin penicillium notatum Penicillum dioscin051016 that insert 100 grams, CCTCC No:M206001 stirs, and under PH4～7 conditions, 26 ℃ fermented 30 hours;
5, filter, filter residue 65 ℃ of dryings, is added the sherwood oil of 300 liters of 80 ℃ of boiling ranges again;
7,60 ℃ of refluxing extraction are 2～3 times, united extraction liquid;
8,60 ℃ of recovery sherwood oil to diosgenin crystallizations are separated out;
9, filter, get the diosgenin crystallization;
10, use 60 ℃ of dissolvings of sherwood oil of 80 ℃ of boiling ranges of diosgenin crystallization double weight, slowly add ethanol again to the solution muddiness, placement is spent the night, recrystallization;
11, leaching crystallization, 60 ℃ of dryings 4 hours, weigh 2.08 kilograms of diosgenins, through efficient liquid phase chromatographic analysis diosgenin content 98.07%.
Claims (1)
1, with yam saponin penicillium notatum Penicillum dioscin 051016, CCTCC No:M206001 prepares the method for diosgenin, it is characterized in that, this method follows these steps to carry out:
A, with the Chinese yam raw material crushing to 5mm;
B, directly 100 ℃ of sterilizations 0.5～1 hour, perhaps add the ammoniacal liquor of raw material weight 0.5%, mix thoroughly, placed 1 hour for 25 ℃～28 ℃;
C, 25 ℃～28 ℃ yam saponin penicillium notatum Penicillumdioscin 051016 that insert raw material weight 0.1%, CCTCC No:M206001 stirs, and under PH4～7 conditions, 25 ℃～28 ℃ fermented 24～36 hours;
The water of d, 4 times of weight of adding fermentation materials;
E, stirring, filtration 60 ℃～70 ℃ dryings, add the sherwood oil of 60 ℃～90 ℃ of boiling ranges of 3～5 times of filter residue weight with filter residue again, 60 ℃ of refluxing extraction 2～3 times, united extraction liquid;
F, 60 ℃ of recovery sherwood oil to diosgenin crystallizations are separated out, and filter, and get the diosgenin crystallization;
60 ℃ of dissolvings of sherwood oil of 60 ℃～90 ℃ of boiling ranges of g, usefulness diosgenin crystallization double weight slowly add ethanol again to the solution muddiness, and placement is spent the night, recrystallization;
H, leaching crystallization, 60 ℃ of dryings obtain the diosgenin crystallization.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101245158A CN100572553C (en) | 2006-09-14 | 2006-09-14 | Method with preparing dioscin with dioscin penicillium notatum |
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| CNB2006101245158A CN100572553C (en) | 2006-09-14 | 2006-09-14 | Method with preparing dioscin with dioscin penicillium notatum |
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| CN100572553C true CN100572553C (en) | 2009-12-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642682A (en) * | 2013-12-20 | 2014-03-19 | 湖北民族学院 | High-efficiency biological reactor and dioscin high-efficiency biological hydrolysis method |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586379A (en) * | 2012-02-15 | 2012-07-18 | 陕西省环境科学研究院 | Water-saving production process of turmeric saponin |
| CN107177662A (en) * | 2017-07-12 | 2017-09-19 | 西北农林科技大学 | The fermentation preparation of Chinese yam saponin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1188425C (en) * | 2002-12-09 | 2005-02-09 | 吉林天药科技股份有限公司 | Novel process for preparing diosgenin |
| CN1228344C (en) * | 2002-10-21 | 2005-11-23 | 吉林天药科技股份有限公司 | Method for preparing yam saponin, medicinal preparation and new usage in medication |
| CN1724685A (en) * | 2005-07-11 | 2006-01-25 | 天津大学 | Method of extracting diosgenin by bioenzyme gradient catalysis |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1228344C (en) * | 2002-10-21 | 2005-11-23 | 吉林天药科技股份有限公司 | Method for preparing yam saponin, medicinal preparation and new usage in medication |
| CN1188425C (en) * | 2002-12-09 | 2005-02-09 | 吉林天药科技股份有限公司 | Novel process for preparing diosgenin |
| CN1724685A (en) * | 2005-07-11 | 2006-01-25 | 天津大学 | Method of extracting diosgenin by bioenzyme gradient catalysis |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642682A (en) * | 2013-12-20 | 2014-03-19 | 湖北民族学院 | High-efficiency biological reactor and dioscin high-efficiency biological hydrolysis method |
| CN103642682B (en) * | 2013-12-20 | 2014-12-17 | 湖北民族学院 | High-efficiency biological reactor and dioscin high-efficiency biological hydrolysis method |
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| CN1932030A (en) | 2007-03-21 |
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