CN1264550C - Chinese medicine resina draconis extract preparing method - Google Patents
Chinese medicine resina draconis extract preparing method Download PDFInfo
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- CN1264550C CN1264550C CN 03151455 CN03151455A CN1264550C CN 1264550 C CN1264550 C CN 1264550C CN 03151455 CN03151455 CN 03151455 CN 03151455 A CN03151455 A CN 03151455A CN 1264550 C CN1264550 C CN 1264550C
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Abstract
The present invention relates to a preparation method for a Chinese medicine of a resina draconis extractive which is provided with the activity of alpha-glycosidase inhibitors. The present invention belongs to the chemical technical field of preparing Chinese herbal medicines. The present invention is characterized by adopting an organic organic-phase polarity gradient extraction method which has the following processes and steps: a raw material-Chinese medicine resina draconis is properly pulverized and dried; then four-step Sorby's extraction orderly using petroleum ether, chloroform, ethyl acetate and propanone is carried out to the resina draconis; the solvent of the four step extractive is thoroughly volatilized by a rotatory evaporator, and the extractive is put on a freeze drier and is changed into powder through freeze drying; the solvent of which the total amount is 5 times of the weight of the raw material resina draconis is extracted; the extraction temperatures are 90 DEG C, 70 DEG C, 90 DEG C and 70 DEG C in turns; the extraction time respectively is 48 hours, 72 hours, 72 hours and 48 hours; finally, all the extractive of the Chinese medicing resina draconis is obtained. The extractive has high inhibitory activity of alpha-glucosaccharase, which is far higher than the inhibitory activity of the existing hypoglycemic medicines. The method has simple technology and convenient operation.
Description
Technical field
The present invention relates to a kind of preparation method, belong to Chinese herbal medicine and prepare technical field of chemistry with Chinese medicine Sanguis Draxonis extract of alpha-glucosidase inhibitor activity.
Background technology
Diabetes are a kind of complex diseases because of syndrome, be that hormone owing to insulin deficit in the body or antagonism insulin increases or can not bring into normal play in target cell a kind of syndrome of glucose, protein and lipid metabolic disorder that physiological action causes of insulin.Present antidiabetic drug polyphyly chemical synthetic drug, kind surplus in the of following 30 can not be divided into three major types, promptly yellow ureas, biguanides and alpha-glucosidase inhibitor.Alpha-glucosidase belongs to the oligosaccharide hydrolase, comprises maltase, isomaltase, saccharase and trehalase etc.Alpha-glucosidase can be alpha-glucose-based from the non-reducing end catalyzing hydrolysis that contains α-glycosidic bond substrate, as hydrolyzing alpha-1, and the α of 4-glycosidic bond and glycogen-1,4-and α-1, the 6-glycosidic bond.And the main hydrolytic enzyme such as maltase by suppressing to be present in mucous membrane of small intestine microvillose membrane surface and saccharase of alpha-glucosidase inhibitor, hinder saccharide compound and resolve into monosaccharide such as glucose, and then play hypoglycemic effect, mainly represent medicine that acarbose (Acarbose) and voglibose (Voglibose) are arranged, both are chemical synthetic drug, inhibition mechanism is competitive inhibitor, can combine with substrate while and enzyme competitiveness, may cause postprandial hypoglycemia.Therefore, seek a kind of hypoglycemic drug safely and effectively, have important clinical application value for treatment, prevention non-insulin-dependent diabetes mellitus, hyperlipemia, obesity, hyperlipoproteinemia.The patent No. is that 98110688.9 Chinese invention patent has been reported a kind of Sanguis Draxonis Chinese medicine preparation that is used for the treatment of diabetes and preparation method thereof, but it only rests on animal and human's body test aspect of the full powder of direct use Sanguis Draxonis, Sanguis Draxonis is not carried out further separation and Extraction, do not relate to the alpha-glucosidase that from Sanguis Draxonis, extracts the tool hypoglycemic activity and suppress composition.
Sanguis Draxonis is the precious Chinese medicine that is described as " panacea of invigorating blood circulation ", and its nature and flavor are sweet, warm, salty, flat, has the effect that blood circulation promoting and blood stasis dispelling, reducing swelling and alleviating pain, hemostasis are enriched blood concurrently.Modern medicine study proves that Sanguis Draxonis has the body of improvement microcirculation, adjusts metabolism, improves effects such as immunologic function.Sanguis Draxonis is mainly derived from the resin of Palmae Daemonorops liana and Liliaceae dracaena plant and belongs to stripping or excretory red resin in its kind of plant fruit together.
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine Sanguis Draxonis extract with hypoglycemic activity, this extract has tangible alpha-glucosidase and suppresses active.
Another object of the present invention is a kind of method of extracting the Sanguis Draxonis effective extract from raw material Chinese medicine Sanguis Draxonis.
The preparation method of a kind of Chinese medicine Sanguis Draxonis extract of the present invention, it is characterized in that adopting organic facies polarity gradient extraction, its process and step are as follows: after suitable pulverizing of raw material Chinese medicine Sanguis Draxonis process and drying, carry out the Soxhlet extracting of four steps successively with petroleum ether, chloroform, ethyl acetate, acetone, with four kinds of solvent extractable matters with Rotary Evaporators with solvent evaporates clean after, add water and place and carry out lyophilization on the freezer dryer to powder; Chinese medicine Sanguis Draxonis quality is 1g: 4ml with the ratio of the total consumption volume of solvent, and each solvent adds with equivalent; Extract temperature and be followed successively by 90 ℃, 70 ℃, 90 ℃, 70 ℃; Extraction time was respectively 48 hours, 72 hours, 72 hours and 48 hours whole Chinese medicine Sanguis Draxonis extract of final acquisition.It is to carry out in apparatus,Soxhlet's that Soxhlet extracts, and adds solvent from the condensing tube upper end, and heats in the water-bath of uniform temperature, makes the continuous reflux, extract, of solvent.
The prepared Chinese medicine Sanguis Draxonis extract of the inventive method possesses higher alpha-glucosidase and suppresses active, and is higher than existing hypoglycemic drug far away; This product safety is nontoxic, is suitable as drug use.This method technology is simple, and is easy to operate.
Now the every performance test result of extract of the present invention is described in the back:
One, Sanguis Draxonis extract is external suppresses vitality test to alpha-glucosidase
The Chinese medicine Sanguis Draxonis extract that adds alpha-glucosidase and various dose in test tube is respectively measured its inhibition activity to alpha-glucosidase.Do positive control with the glucobay (acarbose) (effective ingredient is acarbose) that Bayer A.G produces.Its test result is in following table 1:
Table 1 Sanguis Draxonis inhibitor is to the inhibition activity of alpha-glucosidase
| Inhibitor | Dosage (μ g) | Suppression ratio (%) | ID 50 | Rejection ratio vigor (Unit/mg) |
| The full powder Acarbose of first step extract (ligroin extraction) second step extract (chloroform extract) the 3rd step extract (ethyl acetate extract) the 4th step extract (acetone extract) dragon's blood | 8 16 24 32 40 8 16 24 32 40 2 4 6 8 10 2 4 6 8 10 2 4 6 8 10 24 32 40 1000 2000 3000 4000 | 8.9 10.6 12.0 13.4 15.5 19.1 31.6 44.4 58.7 65.0 21.4 43.3 65.9 83.0 97.3 24.5 57.6 89.5 96.8 98.8 17.5 25.4 41.3 62.3 78.4 85.5 89.3 97.7 31.5 70.2 79.1 82.5 | 0.4g 25.7μg 4.10μg 3.24μg 5.86μg 1.452mg | 3.45 21.209 27.014 15.01 0.075 |
By table 1 as seen, extract after full powder of homemade Guangxi Sanguis Draxonis and all kinds of solvents thereof extract successively all has the inhibition effect to alpha-glucosidase, wherein, homemade Guangxi Sanguis Draxonis the 4th step extract (acetone extract) is the strongest to the inhibition activity of alpha-glucosidase, ID50 reaches 3.24 μ g, only needs 8 μ g and will reach 100% suppression ratio.Each inhibitor ability is followed successively by in the test: the 4th step extract (acetone extract)＞the 3rd step of Guangxi Sanguis Draxonis extract (ethyl acetate extract)＞full powder of domestic Dragon Blood＞second step extract (chloroform extract)＞glucobay (acarbose)＞first step extract (ligroin extraction).The chloroform extract of domestic Dragon Blood has inhibitory action to alpha-glucosidase, but the inhibition vigor is lower, and the ligroin extraction of domestic Dragon Blood does not suppress vigor substantially.Sanguis Draxonis extract of the present invention has very strong alpha-glucosidase and suppresses active, and wherein to suppress activity be 300-380 times of hypoglycemic medicine glucobay (acarbose) to the Sanguis Draxonis acetone extract, has important actual benefit and economic benefit.
Two, the influence of normal mouse fasting glucose is tested
Kunming mouse, body weight 20-22g is divided into 5 groups, and promptly negative control group, positive controls, the 4th step extract are dosage group and acetone extract high dose group in acetone extract low dose group, the acetone extract.Negative control group is irritated the stomach normal saline, and positive controls is irritated stomach and visitd sugared duckweed 50mg/kg, and the acetone extract low dose group is irritated stomach extract 300mg/kg, and middle dosage group is irritated stomach extract 400mg/kg, and high dose group is irritated stomach extract 500mg/kg.Successive administration 7 days, fasting 10h after the last administration, the eye socket venous sinus is got blood, and centrifuging and taking serum is pressed the determination of glucose oxidase blood sugar level, the results are shown in Table 2.
The 4th step of table 2 Sanguis Draxonis extract is to the influence of normal mouse carbohydrate tolerance
| Group | Dosage (mg/kg) | N | Blood glucose value (mmol/L) |
| Negative control group | - | 8 | 4.38±0.98 |
| Positive controls | 50 | 8 | 4.10±0.74 * |
| The acetone extract low dose group | 300 | 7 | 4.30±1.17 * |
| Dosage group in the acetone extract | 400 | 8 | 4.12±0.83 * |
| The acetone extract high dose group | 500 | 7 | 4.21±1.04 * |
* P＜0.01v.s. negative control group
As seen from table, the 4th step of Sanguis Draxonis extract, promptly the middle and high dosage group of acetone extract approaches the Herba Marsileae Quadrifoliae of perforing the formal wedding ceremony to the carbohydrate tolerance effect of normal mouse.
Three, the inductive blood glucose in diabetic mice value test of alloxan Alloxan
Kunming mouse, body weight 20-22g, fasting 24h, lumbar injection Alloxan200mg/kg, once a day, fasting 10h behind the 72h, venous sinus get blood centrifuging and taking determination of serum blood glucose value, choose blood glucose value and experimentize the above person of 11.1mmol/L.The difference of each treated animal average blood sugar value is not more than 0.5mmol/L during grouping.Mice is divided into 5 groups, and promptly negative control group, positive controls, the 4th step of Sanguis Draxonis extract are acetone extract low dose group, middle dosage group and high dose group.Negative control group is irritated the stomach normal saline, and positive controls is irritated stomach and visitd sugared duckweed 50mg/kg, and the 4th step extract is that the acetone extract low dose group is irritated stomach extract 300mg/kg, and middle dosage group is irritated stomach extract 400mg/kg, and high dose group is irritated stomach extract 500mg/kg.Successive administration 10d, fasting 10h after the last administration, the eye socket venous sinus is got blood, and centrifuging and taking serum is pressed the determination of glucose oxidase blood sugar level, the results are shown in Table 3.
The 4th step of table 3 Sanguis Draxonis extract is to the influence of the inductive blood glucose in diabetic mice value of Alloxan
| Group | Dosage (mg/kg) | N | Blood glucose value (mmol/L) |
| Negative control group | - | 7 | 25.83±3.52 |
| Positive controls | 50 | 8 | 15.32±4.10 * |
| The acetone extract low dose group | 300 | 7 | 17.83±2.85 * |
| Dosage group in the acetone extract | 400 | 7 | 15.40±3.21 * |
| The acetone extract high dose group | 500 | 8 | 15.63±3.05 * |
* P＜0.01v.s. negative control group
As seen from table, the middle and high dosage group of Sanguis Draxonis the 4th step extract (being acetone extract) approaches the Herba Marsileae Quadrifoliae of perforing the formal wedding ceremony to the inductive diabetic mice blood sugar decreasing effect of Alloxan.
The specific embodiment
Embodiment one: adopt organic facies polarity gradient extraction, i.e. solvent Soxhlet extracting prepares the Chinese medicine Sanguis Draxonis extract.At first take by weighing the Guangxi Sanguis Draxonis sample 1000g of dry and porphyrize, in the immigration filtration paper cylinder, filtration paper cylinder is put into special Soxhlet extractor, the lower end connects exsiccant 2000ml boiling flask A, add petroleum ether by the condensing tube upper end, dosage is 1000ml, heating makes the continuous reflux, extract, of petroleum ether in 90 ℃ of water-baths, after the extracting 48 hours, take out filtration paper cylinder, wave to the greatest extent wherein solvent, step extraction back residue (Petroleum ether extraction residue) 946g wins, filtration paper cylinder is put into Soxhlet extractor once more, the solvent flask A of Soxhlet extractor lower end is replaced by flask B, add chloroform 1000ml by the condensing tube upper end, heating makes the continuous reflux, extract, of chloroform in 70 ℃ of water-baths, after the extracting 72 hours, take out filtration paper cylinder, wave to the greatest extent wherein solvent, get second step extraction back residue (chloroform extraction residue) 545g, filtration paper cylinder is put into Soxhlet extractor once more, the solvent flask B of Soxhlet extractor lower end is replaced by flask C, add ethyl acetate 1000ml by the condensing tube upper end, heating makes the continuous reflux, extract, of ethyl acetate in 90 ℃ of water-baths, after the extracting 72 hours, take out filtration paper cylinder, wave to the greatest extent wherein solvent, get the 3rd step extraction back residue (ethyl acetate extraction residue) 190g, filtration paper cylinder is put into Soxhlet extractor once more, the solvent flask C of Soxhlet extractor lower end is replaced by flask D, add acetone 1000ml by the condensing tube upper end, heating makes the continuous reflux, extract, of acetone in 90 ℃ of water-baths, after the extracting 48 hours, take out filtration paper cylinder, wave to the greatest extent wherein solvent, get the 4th step extraction back residue (acetone extraction residue) 9g, with solvent flask A, B, content among C and the D uses Rotary Evaporators to concentrate respectively, obtains Sanguis Draxonis ligroin extraction 52g respectively, chloroform extract 396g, ethyl acetate extract 351g and acetone extract 178g.
Claims (2)
1. the preparation method of a Chinese medicine Sanguis Draxonis extract, it is characterized in that adopting organic facies polarity gradient extraction, its process and step are as follows: after suitable pulverizing of raw material Chinese medicine Sanguis Draxonis process and drying, carry out the Soxhlet extracting of four steps successively with petroleum ether, chloroform, ethyl acetate, acetone, with four kinds of solvent extractable matters with Rotary Evaporators with solvent evaporates clean after, add water and place and carry out lyophilization on the freezer dryer to powder; The quality of Chinese medicine Sanguis Draxonis is 1g: 4ml with the ratio of the total consumption volume of solvent, and each solvent adds with equivalent; Extract temperature and be followed successively by 90 ℃, 70 ℃, 90 ℃, 70 ℃; Extraction time was respectively 48 hours, 72 hours, 72 hours and 48 hours whole Chinese medicine Sanguis Draxonis extract of final acquisition.
2. the preparation method of a kind of Chinese medicine Sanguis Draxonis extract according to claim 1, it is characterized in that described Soxhlet extracting is to carry out in apparatus,Soxhlet's, add solvent from the condensing tube upper end, and in the water-bath of uniform temperature, heat, make the continuous reflux, extract, of solvent.
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| CN 03151455 CN1264550C (en) | 2003-09-29 | 2003-09-29 | Chinese medicine resina draconis extract preparing method |
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| CN 03151455 CN1264550C (en) | 2003-09-29 | 2003-09-29 | Chinese medicine resina draconis extract preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1317005C (en) * | 2005-07-28 | 2007-05-23 | 上海大学 | Dragon's blood extract with alpha-glycosidase inhibiting activity and its prepn making process and use |
| CN108853299A (en) * | 2018-07-12 | 2018-11-23 | 云南茶农生物产业有限责任公司 | A kind of extracting method of dragon's blood |
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Granted publication date: 20060719 Termination date: 20091029 |