CN1560061A - Extraction method of Chinese yam extract Huayam saponin - Google Patents
Extraction method of Chinese yam extract Huayam saponin Download PDFInfo
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- CN1560061A CN1560061A CNA2004100168390A CN200410016839A CN1560061A CN 1560061 A CN1560061 A CN 1560061A CN A2004100168390 A CNA2004100168390 A CN A2004100168390A CN 200410016839 A CN200410016839 A CN 200410016839A CN 1560061 A CN1560061 A CN 1560061A
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Abstract
本发明涉及中草药材怀山药提取物怀山药皂甙的提取方法，属中草药化学提炼制备技术领域。本发明怀山药皂甙的提取方法为：怀山药经粉碎后用冷甲醇浸泡，然后过滤，将滤液浓缩，得到的浸膏制成水悬浮液，经脱脂萃取，再用水饱和正丁醇萃取，经再次浓缩后的浸膏，用热的甲醇配制成饱和溶液，然后放置于冰箱内，将析出的沉淀物用蒸馏水溶解，上大孔径吸附树脂，然后收集、浓缩得白色无定型粉末，其主要成分既是怀山药皂甙。该制备物可作为制备降血糖药物和治疗糖尿病并发症药物的主要活性成分或主要原料。The invention relates to a method for extracting Chinese yam saponin from Chinese herbal medicinal material Huayam yam, and belongs to the technical field of chemical extraction and preparation of Chinese herbal medicines. The extraction method of Chinese yam saponin of the present invention is as follows: Chinese yam is soaked with cold methanol after crushing, then filtered, the filtrate is concentrated, and the obtained extract is made into a water suspension, extracted by degreasing, then extracted with water-saturated n-butanol, The concentrated extract is prepared into a saturated solution with hot methanol, then placed in a refrigerator, dissolved in distilled water, and applied to a large-pore adsorption resin, then collected and concentrated to obtain a white amorphous powder, the main component of which is Both Chinese yam saponins. The preparation can be used as the main active ingredient or main raw material for preparing hypoglycemic drugs and drugs for treating diabetic complications.
Description
Technical field
The present invention relates to the extracting method of Chinese medicinal herbs RHIIZOMA DIOSCOREAE frOm Henan of China extract RHIIZOMA DIOSCOREAE frOm Henan of China saponin, belong to the herbal medicine chemistry and refine preparing technical field.
Background technology
Medicinal RHIIZOMA DIOSCOREAE frOm Henan of China is a Dioscoreaceae plant Chinese yam, medicinal part is a rhizome, main chemical compositions has: mannosans, wallantoin, Dopamine HCL, Chinese yam alkali, phytic acid, acerin II and 16 seed amino acids, also contain compositions such as starch, tannin, mucus juice, glycoprotein, polyphenoloxidase, cholesterol, ergosterol, β-Gu Zaichun, Brassicasterin and saponin class, still contain multiple inorganic elementss such as iodine, phosphorus, calcium in addition.
RHIIZOMA DIOSCOREAE frOm Henan of China saponin in the RHIIZOMA DIOSCOREAE frOm Henan of China extract has alpha-glucoside inhibiting activity, has hexokinase to activate activity and aldose reductase inhibition activity simultaneously, so can be used as hypoglycemic drug treatment diabetes and complication thereof.
Summary of the invention
The objective of the invention is to extract a kind of method by crude drug bosom medicament extract RHIIZOMA DIOSCOREAE frOm Henan of China saponin.
The purpose of this invention is to provide a kind of alpha-glucoside inhibiting activity that both had, have aldose reductase inhibition activity and hexokinase again and activate active RHIIZOMA DIOSCOREAE frOm Henan of China extract, its significant part is the water-soluble RHIIZOMA DIOSCOREAE frOm Henan of China saponin with good hypoglycemic activity.
The objective of the invention is to reach by the following technical programs.
The extracting method of a kind of RHIIZOMA DIOSCOREAE frOm Henan of China extract RHIIZOMA DIOSCOREAE frOm Henan of China saponin of the present invention is characterized in that this method comprises following processing step:
A. the crude drug RHIIZOMA DIOSCOREAE frOm Henan of China is extracted with the methyl alcohol cold soaking through after pulverizing, and extraction time is 10-24 hour, extracts twice altogether, and its solvent load is 3-5 a times of crude drug;
B. filter then, filtrate concentrates with Rotary Evaporators, and temperature is controlled to be about 30-50 ℃, obtains medicinal extract after concentrating;
C. medicinal extract is positioned in the 200ml-300ml distilled water, makes it become aqeous suspension;
D. aqeous suspension is extracted 2-3 time with the anhydrous diethyl ether degreasing;
E. will extract 2-3 time with the propyl carbinol saturation water through the water layer after the anhydrous diethyl ether degreasing extraction;
F. collect the extraction liquid of water-saturated n-butanol, be positioned in the Rotary Evaporators and concentrate, temperature is controlled at 50 ℃, concentrate and medicinal extract;
G. above-mentioned medicinal extract is dissolved the state that reaches capacity with hot methanol, in 0-4 ℃ refrigerator, placed 3 days then, obtain the oyster white crystallization;
H. with above-mentioned crystallization dissolved in distilled water, last macroporous type polymeric adsorbent, first distilled water wash-out with 2-5 times of chromatography column volume, use 20% ethanol, 70% ethanol, dehydrated alcohol wash-out successively again, collect 70% alcoholic acid elutriant, put into Rotary Evaporators heat concentrated, then with its lyophilize
Last main component is the oyster white amorphous powder of RHIIZOMA DIOSCOREAE frOm Henan of China saponin.
The RHIIZOMA DIOSCOREAE frOm Henan of China saponin that aforesaid method makes, has alpha-glucoside inhibiting activity, its mechanism of action be the RHIIZOMA DIOSCOREAE frOm Henan of China saponin by with digestive tube in many enzyme effects, particularly to the inhibition activity of alpha-glycosidase, thereby controlled the absorption of body, made it have anti-trophicity nutritive ingredients such as glucose.It is active that the RHIIZOMA DIOSCOREAE frOm Henan of China saponin has the hexokinase activation simultaneously, thereby accelerated the degraded of sugar in the carbohydrate metabolism approach.For the patient of the eye pathology in the diabetic complication, DPN and kidney portion pathology, RHIIZOMA DIOSCOREAE frOm Henan of China also has aldose reductase inhibition activity, thereby can eliminate accumulating of the interior sorbyl alcohol of body, so the RHIIZOMA DIOSCOREAE frOm Henan of China saponin can be used as the medicine of treatment diabetes and complication thereof.
Extraction process of the present invention, use equipment is simple, the separation and Extraction processing ease.
Embodiment
Specific embodiments of the invention as mentioned above, existing be described in detail again in after.
Concrete processing step in the present embodiment is as follows:
A. take by weighing crude drug RHIIZOMA DIOSCOREAE frOm Henan of China 1000 gram (siccative), after pulverizing, get with the methyl alcohol lixiviate, cold soaking extraction time is 24 hours, extracts twice altogether, and quantity of solvent is 3-5 a times of crude drug;
B. filter then, filtrate is concentrated with Rotary Evaporators, the temperature during rotary evaporation is controlled at 45 ℃, obtains medicinal extract after concentrating;
C. medicinal extract is positioned in the 300ml distilled water, makes it become aqeous suspension;
D. aqeous suspension is extracted 2 times with the dehydrated alcohol degreasing in separating funnel;
E. the water liquid layer that will collect after dehydrated alcohol degreasing extraction concentrates in separating funnel, and Heating temperature is 50 ℃;
F. collect the extraction liquid of water-saturated n-butanol, be positioned in the Rotary Evaporators and concentrate, temperature is controlled at 50 ℃, concentrate and medicinal extract;
G. above-mentioned medicinal extract is dissolved the state that reaches capacity with hot methanol, in 0-4 ℃ refrigerator, placed 3 days then, obtain the oyster white crystallization;
H. with above-mentioned crystallization dissolved in distilled water, last macroporous type polymeric adsorbent, first distilled water wash-out with 2-5 times of chromatography column volume, use 20% ethanol, 70% ethanol, dehydrated alcohol wash-out successively again, collect 70% alcoholic acid elutriant, put into Rotary Evaporators and heat concentratedly, then with its lyophilize, last main component is the oyster white amorphous powder of RHIIZOMA DIOSCOREAE frOm Henan of China saponin.
In order to illustrate that prepared product RHIIZOMA DIOSCOREAE frOm Henan of China saponin of the present invention can reduce the effect of blood blood sugar concentration, the spy has done some relevant tests
One, the RHIIZOMA DIOSCOREAE frOm Henan of China saponin is to zymetology effect in the hypoglycemic activity of animal mouse and the body.
Test 1: RHIIZOMA DIOSCOREAE frOm Henan of China saponin single administration is to the influence of normal mouse's blood sugar content: get 50 of normal mouses, be divided into 5 groups at random, irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), RHIIZOMA DIOSCOREAE frOm Henan of China saponin (30mg/kg, 60mg/kg, 100mg/kg) respectively.Hematometry blood plasma blood sugar concentration is got in docking behind the fasting 4h.The results are shown in Table 1.
Table 1 RHIIZOMA DIOSCOREAE frOm Henan of China saponin single administration is to the influence of normal mouse's blood sugar content
| Group | ????n | Dosage (mg/kg) | Blood glucose value (mmol/L) |
| Physiological saline | ????10 | ????- | ??9.21±0.67 |
| Glucobay (acarbose) | ????10 | ????100 | ??6.76±0.51 1 |
| The RHIIZOMA DIOSCOREAE frOm Henan of China saponin | ????10 ????10 ????10 | ????30 ????60 ????100 | ??7.78±0.64 1??7.38±1.14 1??6.84±0.32 1 |
Compare with the physiological saline group:
1P＜0.005
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product
Above-mentioned test-results shows that RHIIZOMA DIOSCOREAE frOm Henan of China saponin 30mg/kg, 60mg/kg, 100mg/kg dosage all can obviously reduce normal mouse blood sugar.
Test 2, the administration of RHIIZOMA DIOSCOREAE frOm Henan of China saponin continuous several times are to the influence of normal mouse's blood sugar content: get 30 of normal mouses, be divided into 3 groups at random, irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), RHIIZOMA DIOSCOREAE frOm Henan of China saponin (100mg/kg) respectively, continuous eight days.Fasting 4h after the last administration, hematometry blood plasma blood sugar concentration is got in docking.By the result of table 2 as seen,
The administration of table 2 RHIIZOMA DIOSCOREAE frOm Henan of China saponin continuous several times is to the influence of normal mouse's blood sugar content
| Group | ????N | Blood glucose value (mmol/L) |
| Physiological saline | ????10 | ????7.22±0.53 |
| Glucobay (acarbose) | ????10 | ????5.59±0.53 1 |
| The RHIIZOMA DIOSCOREAE frOm Henan of China saponin | ????10 | ????5.65±0.82 1 |
Compare with the physiological saline group:
1P＜0.005
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product
Above-mentioned experimental result shows, the RHIIZOMA DIOSCOREAE frOm Henan of China saponin can cause the reduction of normal mouse blood sugar equally to this administration, and its effect is suitable with commercially available ofhypoglycemic medicine glucobay (acarbose).
Test 3: the RHIIZOMA DIOSCOREAE frOm Henan of China saponin is to the influence of alloxan diabetes mouse's blood sugar content: 35 of alloxan diabetes mouse, be divided into 3 groups (blood glucose value difference is no more than 0.1mmol/L between group), irritate stomach physiological saline, glucobay (acarbose) (100mg/kg), RHIIZOMA DIOSCOREAE frOm Henan of China saponin (100mg/kg) respectively, continuous eight days.Fasting 4h after the last administration gets hematometry blood plasma blood sugar concentration.It the results are shown in Table 3.
Table 3 RHIIZOMA DIOSCOREAE frOm Henan of China saponin is to the influence of alloxan diabetes mouse's blood sugar content
| Group | ????n | Blood glucose value (mmol/L) |
| Physiological saline | ??10 | ?11.25±0.93 |
| Glucobay (acarbose) | ??10 | ?8.38±1.10 1 |
| The RHIIZOMA DIOSCOREAE frOm Henan of China saponin | ??15 | ?8.21±1.02 1 |
Compare with the physiological saline group:
1P＜0.005
Above-mentioned glucobay (acarbose) contrast agents is Bayer A.G's product
Above-mentioned test-results shows that the RHIIZOMA DIOSCOREAE frOm Henan of China saponin can effectively reduce the blood sugar of alloxan diabetes mouse, and under Isodose, its effect slightly is better than orally-taken blood sugar reducing medicine glucobay (acarbose).
Test 4: the influence that the RHIIZOMA DIOSCOREAE frOm Henan of China saponin is lived to mouse body endoenzyme: with each 10 of normal mouse and alloxan diabetes mouse, irritate stomach physiological saline, again 15 of alloxan diabetes mouse are irritated stomach RHIIZOMA DIOSCOREAE frOm Henan of China saponin (100mg/kg), continuous eight days.Fasting 4h after the last administration gets behind the blood head-breaking and puts to death, and measures alpha-glucosidase, hexokinase and aldose reductase activity in the body, the results are shown in Table 4.
Table 4 RHIIZOMA DIOSCOREAE frOm Henan of China saponin is in the intravital enzyme effect of mouse
| Group | Absorbance | Inhibiting rate | Activity ratio | |
| Alpha-glucosidase | The physiological saline group | ??0.487±0.119 | ??26.21％ | |
| Diabetic model group | ??0.454±0.170 | |||
| The administration group | ??0.335±0.077 1 | |||
| Hexokinase | The physiological saline group | ??0.038±0.007 | ??27.50％ | |
| Diabetic model group | ??0.040±0.009 | |||
| The administration group | ??0.051±0.013 1 | |||
| Aldose reductase | The physiological saline group | ??0.091±0.009 | ??13.16％ | |
| Diabetic model group | ??0.114±0.014 2 | |||
| The administration group | ??0.099±0.011 1 |
Compare with the physiological saline group:
2P＜0.05
Compare with diabetic model group:
1P＜0.05.
Test-results shows:
1. diabetic model group and physiological saline group (normal mouse) are comparatively speaking, change in the activity of alpha-glucosidase and hexokinase, and the activity of aldose reductase has obvious rising (enzyme absorbance alive rises 0.023), illustrates that hyperglycemia can activate aldose reductase.
2. administration group and diabetic model group are comparatively speaking, the activity of alpha-glucosidase has obvious inhibition (inhibiting rate is 26.21%), the activity of aldose reductase also is suppressed (inhibiting rate position 13.16), the activity of hexokinase then be activated (activity ratio is 27.50%)
By above each test, generally speaking, prepared product RHIIZOMA DIOSCOREAE frOm Henan of China saponin of the present invention has alpha-glucosidase inhibition activity in the body to experiment mice, and the activation activity of hexokinase is arranged simultaneously, and the inhibition activity of aldose reductase.
Claims (2)
1. the extracting method of a RHIIZOMA DIOSCOREAE frOm Henan of China extract RHIIZOMA DIOSCOREAE frOm Henan of China saponin is characterized in that this method has following technological process and processing step:
A. starting material crude drug RHIIZOMA DIOSCOREAE frOm Henan of China is got with methyl alcohol and/or water-cooled lixiviate through after pulverizing, and extraction time is 10-24 hour, extracts twice altogether, and solvent load is 3-5 a times of crude drug;
B. filter then, filtrate concentrates with Rotary Evaporators, and temperature is controlled at about 30-50 ℃, obtains medicinal extract after concentrating;
C. medicinal extract is suspended in the 200-300ml distilled water, makes it become aqeous suspension;
D. the water layer after anhydrous diethyl ether degreasing extraction extracts 2-3 time with the propyl carbinol saturated aqueous solution;
E. collect the extraction liquid of water-saturated n-butanol, be positioned in the Rotary Evaporators and concentrate, temperature is controlled at about 40-50 ℃, concentrate and medicinal extract;
F. above-mentioned medicinal extract is dissolved the state that reaches capacity with hot methanol, in 0-4 ℃ refrigerator, placed 3 days then, obtain the oyster white crystallization;
G. with above-mentioned crystallization dissolved in distilled water, last macroporous type polymeric adsorbent, first distilled water wash-out with 2-5 times of chromatography column volume, use 20% ethanol, 70% ethanol, dehydrated alcohol wash-out successively again, collect 70% alcoholic acid elutriant, put into Rotary Evaporators and heat concentratedly, then with its lyophilize, obtaining main component at last is the oyster white amorphous powder of RHIIZOMA DIOSCOREAE frOm Henan of China saponin.
2. the RHIIZOMA DIOSCOREAE frOm Henan of China saponin product that extracting method extracted of a kind of RHIIZOMA DIOSCOREAE frOm Henan of China extract RHIIZOMA DIOSCOREAE frOm Henan of China saponin according to claim 1, its purposes can be used as the main active ingredient or the main raw material of preparation hypoglycemic drug and the diabetes complicated disease drug of treatment.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101370394A (en) * | 2005-11-14 | 2009-02-18 | 国立阳明大学 | Chinese yam low molecular weight extract and its preparation method |
| CN101870721A (en) * | 2010-04-30 | 2010-10-27 | 邓振全 | Extraction method of dioscin |
| EP1942920A4 (en) * | 2005-10-28 | 2011-10-19 | Sun-Yeou Kim | EXTRACT FROM THE DIOSCOREACEAE FAMILY AND COMPOSITION COMPRISING SAME FOR PREVENTING OR TREATING PERIPHERAL NEUROPATHY |
| CN103055098A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried yam for preventing and treating cancer |
| CN103055097A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried dioscorea opposita for treating diabetes mellitus |
| CN103520425A (en) * | 2013-10-18 | 2014-01-22 | 广西中医药大学 | Preparation method and application of effective part of dioscorea persimilis for decreasing blood sugar |
| CN108239136A (en) * | 2016-12-26 | 2018-07-03 | 天津延生园生物科技有限公司 | A kind of extracting method of dioscin |
| CN114515006A (en) * | 2022-02-22 | 2022-05-20 | 瑞昌市渝瑞实业有限公司 | Method and system for extracting saponin from Chinese yam to prepare nutrition powder |
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2004
- 2004-03-10 CN CNA2004100168390A patent/CN1560061A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1942920A4 (en) * | 2005-10-28 | 2011-10-19 | Sun-Yeou Kim | EXTRACT FROM THE DIOSCOREACEAE FAMILY AND COMPOSITION COMPRISING SAME FOR PREVENTING OR TREATING PERIPHERAL NEUROPATHY |
| US8202554B2 (en) | 2005-10-28 | 2012-06-19 | Sun-Yeou Kim | Extract of the family dioscoreaceae and composition for preventing or treating peripheral neuropathy comprising the same |
| CN102145105B (en) * | 2005-10-28 | 2013-07-03 | 金善砺 | Extract of the family dioscoreaceae and composition for preventing or treating peripheral neuropathy comprising the same |
| CN101370394A (en) * | 2005-11-14 | 2009-02-18 | 国立阳明大学 | Chinese yam low molecular weight extract and its preparation method |
| CN101370394B (en) * | 2005-11-14 | 2014-12-10 | 国立阳明大学 | Chinese yam low molecular weight extract and its preparation method |
| CN101870721A (en) * | 2010-04-30 | 2010-10-27 | 邓振全 | Extraction method of dioscin |
| CN103055098A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried yam for preventing and treating cancer |
| CN103055097A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried dioscorea opposita for treating diabetes mellitus |
| CN103520425A (en) * | 2013-10-18 | 2014-01-22 | 广西中医药大学 | Preparation method and application of effective part of dioscorea persimilis for decreasing blood sugar |
| CN103520425B (en) * | 2013-10-18 | 2016-03-23 | 广西中医药大学 | The preparation method and its usage of Dioscarea persimilis Prain et Burkill． blood-sugar-lowering effective parts |
| CN108239136A (en) * | 2016-12-26 | 2018-07-03 | 天津延生园生物科技有限公司 | A kind of extracting method of dioscin |
| CN114515006A (en) * | 2022-02-22 | 2022-05-20 | 瑞昌市渝瑞实业有限公司 | Method and system for extracting saponin from Chinese yam to prepare nutrition powder |
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