CN102552791B - Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food - Google Patents
Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food Download PDFInfo
- Publication number
- CN102552791B CN102552791B CN201210010573.3A CN201210010573A CN102552791B CN 102552791 B CN102552791 B CN 102552791B CN 201210010573 A CN201210010573 A CN 201210010573A CN 102552791 B CN102552791 B CN 102552791B
- Authority
- CN
- China
- Prior art keywords
- chloroform
- methanol
- add
- filtrate
- fructus tsaoko
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses an active ingredient extracted from Amomum tsao-ko and application of the ingredient in preparing blood sugar reducing medicine and food. The active ingredient is prepared by extracting Amomum tsao-ko powder in a chloroform-carbinol-water system, passing trough a silica gel column, respectively sequentially eluting by chloroform, acetone and carbinol, passing the carbinol eluent through the silica gel column, and eluting by the chloroform-carbinol-water system. The active ingredient has the function of blood sugar reduction and can be made into blood sugar reducing medicine and blood sugar reducing health food.
Description
Technical field
The present invention relates to a kind of active component extracting and in the application of preparing in blood sugar lowering medicine and food from Fructus Tsaoko.
Technical background
China's diabetics growth rate is rapid, and especially mid-aged population hyperglycemia ratio increases year by year.But the exploitation of China's blood-sugar lowering type health-care food quite lags behind.Hesperian blood-sugar lowering type health-care food has developed into important new industry.The annual blood-sugar lowering type health-care food market sales revenue of the U.S. is up to 2,500,000,000～3,000,000,000 dollars, and kind reaches more than hundreds of.Japan's onset diabetes rate has approached 4%, and its corresponding blood-sugar lowering type health-care food industry also develops rapider, and within 2002, total sales volume just breaks through 1,000,000,000,000 yen, and wherein blood sugar lowering/slimming health food accounts for 1/2 share.And in China, the average attack rate of former diabetes in 1978, lower than 1%, will have risen to 3.4% to the end of the year 2000, between short 20 years, onset diabetes rate has been turned over some.Now, Beijing-Shanghai regional onset diabetes rate has reached even respectively 8% and 11%.Therefore, blood-sugar lowering type health-care food market is huge, and has huge market operation space and consumption demand, and industry benefit is very considerable.International medical community generally believes, diabetes patient not only should take the too high blood glucose of hypoglycemic medicine control, and some Special food (health food) of ingesting can play the effect of controlling hyperglycemia equally.This group food is exactly function of polysaccharide food.
Antihypelipidemic foodstuff in selling on international market at present has at least more than hundreds of, is wherein followed successively by 4 kinds of best blood-sugar lowering type health-care foods of western countries' sales situations such as the U.S.: Fructus Momordicae charantiae (main active is " bitter gourd polypeptide "); India's Largeleaf Gymnema (main component is " gymnemic acid "); Calabash Fructus Crotonis (main component is trigonella bean gum); Cortex Cinnamomi powder (main component is " cinnamic acid ").Although China has been diabetes states occurred frequently, the domestic large market of blood sugar reducing health product that not yet forms.Therefore exploitation new resources blood-sugar lowering type health-care food will have wide market prospect in China.
Fructus Tsaoko (Amomum tsao-ko Crevostet Lemarie) has plantation at wide geographic areas such as Yunnan Province of China, Guangxi, Guizhou, and wide material sources, as food spice and the existing history in thousand of Chinese herbal medicine application.People have identified nearly 80 kinds of chemical compositions from Fructus Tsaoko quintessence oil, are mainly 1,8-cineole, citral, geraniol, trans-2-and-ecenal, 2-decenal, nopinene etc.At present there are no the report about Fructus Tsaoko blood sugar reducing function.
Summary of the invention
The object of this invention is to provide the active component extracting that a kind of hypoglycemic effect is good from Fructus Tsaoko.
Another object of the present invention is to provide above-mentioned active component in the application of preparing in blood sugar lowering medicine and food.
The technical scheme that the present invention takes:
A kind of active component extracting from Fructus Tsaoko, obtain by the following method: after the Fructus Tsaoko peeling of drying, pulverize, with the extraction of chloroform-methanol-aqueous systems, after extraction through removing by filter residue, filtrate is through separatory funnel stratification, take off metafiltration liquid, filtrate obtains saturated concentrated solution at 30-40 DEG C through vacuum concentration, described saturated concentrated solution is passed through to silica dioxide gel post, and use successively respectively chloroform, acetone, methanol-eluted fractions, get meoh eluate and after vacuum concentration becomes saturated solution, cross silica dioxide gel post, carry out eluting as eluant by chloroform-methanol-aqueous systems, collect front 60% eluent extremely saturated through vacuum concentration, put into freezer dryer lyophilization 48-72 hour, obtain active component solids.
In described chloroform-methanol-aqueous systems, the volume ratio of chloroform, first alcohol and water is 5:10:1.
The described active component extracting from Fructus Tsaoko is in the application of preparing in blood sugar reducing health medicine and food interpolation.
The addition of active component described in described application is not less than 0.001 wt %.
The beneficial effect that the present invention adopts technique scheme to obtain: it is raw material that the present invention utilizes China's local product resource Fructus Tsaoko, the active component extracting has significant effect of lowering blood sugar, its hypoglycemic effect is better than Cortex Cinnamomi powder (see figure 1), the crowd who increases for person in middle and old age's blood glucose, the biological preparation that provides effective prevention blood glucose to increase for market, this active component can coordinate with inorganic forming agent or organic forming agent, be deployed into the oral application dosage form of various routines, as: capsule, tablet, oral liquid etc., also in the middle of can making an addition to various food, make various functional antihypelipidemic foodstuffs.
Brief description of the drawings
Fig. 1 is the hypoglycemic effect comparison diagram of Fructus Tsaoko powder and Cortex Cinnamomi powder;
Fig. 2 is that standard feed and the experiment feedstuff that adds Fructus Tsaoko active component suppress body weight increase effect contrast figure;
Fig. 3 is that standard feed and the experiment feedstuff that adds Fructus Tsaoko active component reduce blood sugar concentration effect contrast figure.
Detailed description of the invention
Embodiment 1: the preparation of Fructus Tsaoko active component
(1) dry Fructus Tsaoko is after peeling, be ground into the above powder of 100 order, get 50g Caoguo, add 150ml chloroform, 300ml methanol and 30ml deionized water, at room temperature soak after 12 hours with homogenizer high-speed stirred (revolution 1600-20000 rev/min) 5-10 minute, then use ultrasonic homogenizer homogenizing 10 minutes (power is 500-1000W), leave standstill more than 4 hours, sucking filtration obtains filtrate, filtrate moves to 1L separatory funnel, vibrate and leave standstill 12 hours after 1 minute, chloroform layer (lower floor's night) and methanol layer (upper strata liquid) are separated, upper strata liquid divides and washs rear and subnatant merging for 3 times with 100ml chloroform, mixed liquor after merging adds 2g anhydrous sodium sulfate drying, filter to get filtrate.Filtering residue repeats above-mentioned steps 3-6 time, merges the chloroform layer filtrate of each extraction.
(2), by above-mentioned chloroform layer filtrate, after 30-40 degree is concentrated, put into freezer dryer lyophilization 48-72 hour through Rotary Evaporators.Above-mentioned dried solid adds chloroform/methanol mixed solution (chloroform: methanol=1:2) 200ml to dissolve again, after 1 minute, filter with homogenizer homogenizing, filtrate moves to separatory funnel, after separatory, take off layer chloroform layer liquid after Rotary Evaporators is concentrated below 40 degree, put into freezer dryer lyophilization 48-72 hour.Aforesaid operations repeats 3 times, makes extract I.
(3) by dry 200-300 order silica gel H 500g, the apparent density of dry silica gel is in 0.4 left and right, (chloroform anhydrous calcium chloride is dry to add the chloroform of one times of dry silica gel volume, to remove alcohol and water, fully stir with Glass rod, vacuumize degassing 20 minutes, adopts wet method to fill with post (chromatographic column is the glass column of the long 600ml of diameter 55mm).After sedimentation completes, the superiors add the quartz sand of 1-2cm, add more chloroform, with duplex ball or air pump pressurization, until constant flow rate.Post bed is approximately compressed into 9/10 volume, finally makes with chloroform in 1000ml normal hexane column precipitator the chromatographic column that loading is 55mm × 500mm.
(4) take the extract A 6g obtaining in step (2), adding appropriate absolute methanol to be dissolved into saturated solution slowly adds from chromatographic column upper end, after solvent layer drops to quartz sand bottom surface, carry out eluting with 1200ml chloroform, 1000ml acetone, 1200ml methanol respectively, collect meoh eluate, after Rotary Evaporators is concentrated under 30-40 degree, put into freezer dryer lyophilization 48-72 hour, obtain methanol leachable II.
(5) chloroform 100ml, methanol 100ml, deionized water 30ml are mixed, be made into mixed liquor, then this mixed liquor is diluted to 10 times as eluent with chloroform.Add appropriate methanol to make saturated solution above-mentioned methanol leachable B, slowly add from chromatographic column upper end, after solvent layer drops to quartz sand bottom surface, carry out drip washing with the eluent of above-mentioned preparation, collect the 1500ml eluent starting from chromatographic column effluent, after Rotary Evaporators is concentrated under 30-40 degree, put into freezer dryer lyophilization 48-72 hour, must have the Fructus Tsaoko hypoglycemic activity composition of ultraviolet absorption characteristic, what in remaining eluent, elute is mainly polysaccharide component.
Embodiment 2: the preparation of the experiment feedstuff that contains Fructus Tsaoko active component
Take the component of following mass percent: starch 47.8%, casein 20%, sucrose 15%, Adeps Sus domestica 6%, cellulose 5%, mixed mineral salt 4%, mixed vitamin 2%, METHIONINE 0.2%; Above raw material after sufficiently mixing, is modulated into standard feed.In per kilogram standard feed, add the Fructus Tsaoko hypoglycemic activity composition making in the embodiment 1 of 50-500mg, be mixed with experiment feedstuff.
The ICR male mice random assortment in 40 12 week ages is become to tetra-groups of A, B, C, D, every group 10, A group is matched group, pay standard feedstuff, B group is supplied with the experiment feedstuff that adds methanol leachable II, it is Fructus Tsaoko active component that the component that has ultraviolet absorption characteristic obtaining in front 60% eluent is added in the supply of C group, and D group is supplied with and added the polysaccharide component obtaining in rear 40% eluent.Every per day every mice is supplied with 4.5g feedstuff, feed 90 days, and every day observe mice situation, survey weekly body weight one time, the results are shown in Figure the data difference differnce table 1 that the Spjotvoll/Stoline test statistical analysis of tetra-groups of experimental datas of 2(draws, this test is to draw the in the situation that of P<0.05.) feed and finish after, A group and C group mice are taken a blood sample after carbon dioxide narcosis, blood separates through frozen centrifugation, measurement blood lipid peroxide (TBARS) and blood sugar concentration, experimental result is shown in Fig. 3.
The Spjotvoll/Stoline test results of statistical analysis of table 1 Fig. 2
| My god | A group | B group | C group | D group |
| 60 | b | c | bc | ab |
| 90 | b | c | c | a |
The feedstuff that adds as can be seen from Figure 2 Fructus Tsaoko hypoglycemic activity composition is compared with standard feed and is had the effect that obvious inhibition person in middle and old age Mouse Weight increases, and the material then eluting in 40% eluent obviously can increase the body weight of person in middle and old age mice.As seen from the results in Table 1, working what suppress body weight increasing action is Fructus Tsaoko active component for there being the component of ultraviolet absorption characteristic.The feedstuff that adds as can be seen from Figure 3 Fructus Tsaoko hypoglycemic activity composition is compared with standard feed and is had the blood sugar concentration of obvious reduction person in middle and old age mices (12 weeks more than age).Fructus Tsaoko active component centering Aged Mice of the present invention has the effect that reduces blood glucose value and suppress body weight gain.
Embodiment 3: the preparation of the blood sugar lowering oral formulations that contains Fructus Tsaoko active component
By Fructus Tsaoko hypoglycemic activity composition powder dry 100mg, add the dissolve with ethanol solution of 100ml50%, to be dissolvedly add 100g oligosaccharide as excipient after completely, mix according to a conventional method pelletize, obtain the granular preparations for oral administration of Fructus Tsaoko hypoglycemic activity composition.
Embodiment 4: the preparation of the blood-sugar lowering type health-care food that contains Fructus Tsaoko active component
Get commercially available Sucus Pyri 500ml, add the Fructus Tsaoko hypoglycemic activity composition of embodiment 1 gained of 100mg, fully mix, after sterilization packaging, make and be applicable to the health care Sucus Pyri with blood sugar reducing function that person in middle and old age drink.
Embodiment 5: other steps are with embodiment 4, and difference is that the amount of the Fructus Tsaoko hypoglycemic activity composition adding is 5mg.
Claims (3)
1. the active component extracting from Fructus Tsaoko, is characterized in that it obtains by the following method:
(1) dry Fructus Tsaoko is after peeling, be ground into the above powder of 100 order, get 50g Caoguo, add 150ml chloroform, 300ml methanol and 30ml deionized water, at room temperature soak after 12 hours and under revolution 1600-20000 rev/min, stir 5-10 minute with homogenizer, then be 500-1000W ultrasonic homogenizer homogenizing 10 minutes with power, leave standstill more than 4 hours, sucking filtration obtains filtrate, filtrate moves to 1L separatory funnel, vibrate and leave standstill 12 hours after 1 minute, making chloroform layer is that subnatant is that upper strata liquid separates with methanol layer, upper strata liquid divides and washs rear and subnatant merging for 3 times with 100ml chloroform, mixed liquor after merging adds 2g anhydrous sodium sulfate drying, filter to get filtrate, filtering residue repeats above-mentioned steps 3-6 time, merges the chloroform layer filtrate of each extraction,
(2), by above-mentioned chloroform layer filtrate, after 30-40 degree is concentrated, put into freezer dryer lyophilization 48-72 hour through Rotary Evaporators; Dried solid adds the chloroform/methanol mixed solution 200ml of chloroform: methanol=1:2 to dissolve again, after 1 minute, filter with homogenizer homogenizing, filtrate moves to separatory funnel, after separatory, take off layer chloroform layer liquid after Rotary Evaporators is concentrated below 40 degree, put into freezer dryer lyophilization 48-72 hour; Aforesaid operations repeats 3 times, makes extract I;
(3) by dry 200-300 order silica gel H 500g, the apparent density of dry silica gel is 0.4, add the chloroform of one times of dry silica gel volume, fully stir with Glass rod, vacuumize degassing 20 minutes, chloroform is dry with anhydrous calcium chloride in advance, to remove alcohol and water, adopt wet method to fill with post, chromatographic column is the glass column of the long 600mm of diameter 55mm; After sedimentation completes, the superiors add the quartz sand of 1-2cm, add more chloroform, with duplex ball or air pump pressurization, until constant flow rate; Post bed is compressed into 9/10 volume, finally makes with chloroform in 1000ml normal hexane column precipitator the chromatographic column that loading is 55mm × 500mm;
(4) take the extract I 6g obtaining in step (2), adding appropriate absolute methanol to be dissolved into saturated solution slowly adds from chromatographic column upper end, after solvent layer drops to quartz sand bottom surface, carry out eluting with 1200ml chloroform, 1000ml acetone, 1200ml methanol respectively, collect meoh eluate, after Rotary Evaporators is concentrated under 30-40 degree, put into freezer dryer lyophilization 48-72 hour, obtain methanol leachable II;
(5) chloroform 100ml, methanol 100ml, deionized water 30ml are mixed, be made into mixed liquor, then this mixed liquor is diluted to 10 times as eluent with chloroform; Add appropriate methanol to make saturated solution above-mentioned methanol leachable II, slowly add from chromatographic column upper end, after solvent layer drops to quartz sand bottom surface, carry out drip washing with the eluent of above-mentioned preparation, collect the 1500ml eluent starting from chromatographic column effluent, after Rotary Evaporators is concentrated under 30-40 degree, put into freezer dryer lyophilization 48-72 hour, must there is the Fructus Tsaoko hypoglycemic activity composition of ultraviolet absorption characteristic.
2. the active component extracting from Fructus Tsaoko claimed in claim 1 is in the application of preparing in blood sugar reducing health medicine and blood-sugar lowering type health-care food.
3. application according to claim 2, is characterized in that the addition of described active component is not less than 0.001 wt %.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210010573.3A CN102552791B (en) | 2012-01-14 | 2012-01-14 | Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210010573.3A CN102552791B (en) | 2012-01-14 | 2012-01-14 | Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102552791A CN102552791A (en) | 2012-07-11 |
| CN102552791B true CN102552791B (en) | 2014-06-11 |
Family
ID=46400245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210010573.3A Expired - Fee Related CN102552791B (en) | 2012-01-14 | 2012-01-14 | Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102552791B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634346A (en) * | 2004-10-27 | 2005-07-06 | 上海大学 | Preparation method of amomum fruit volatile oil nanometer liposome turbid liquor medicament |
| CN101347424A (en) * | 2007-07-20 | 2009-01-21 | 复旦大学 | Use of luteolin in preparing anticomplement medicament |
-
2012
- 2012-01-14 CN CN201210010573.3A patent/CN102552791B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634346A (en) * | 2004-10-27 | 2005-07-06 | 上海大学 | Preparation method of amomum fruit volatile oil nanometer liposome turbid liquor medicament |
| CN101347424A (en) * | 2007-07-20 | 2009-01-21 | 复旦大学 | Use of luteolin in preparing anticomplement medicament |
Non-Patent Citations (10)
| Title |
|---|
| #8722 * |
| "Tsaokoin, a New Bicyclic Nonane from Amomum tsao-ko";Qi Shi SONG1,et al.;《Chinese Chemical Letters》;20011231;第12卷(第3期);第227−230页 * |
| "加热回流法提取草果中抗氧化成分的研究";李婷 等;《食品研究与开发》;20090831;第30卷(第8期);第23-26页 * |
| "国产草果化学成分研究进展";马洁 等;《中国中医药信息杂志》;20050930;第12卷(第9期);第97-98页 * |
| 230页. * |
| LongquanYu，et al.."effect of lipid extracted from tsao-ko(amomum tsao-ko crevost et lemaire) on digestive enzyme activity,antioxidant activity, plasma and liver lipids, and blood glucose levels of mice".《J Nutr Sci Vitaminol》.2008,第54卷第378-383页. |
| LongquanYu,et al.."effect of lipid extracted from tsao-ko(amomum tsao-ko crevost et lemaire) on digestive enzyme activity,antioxidant activity, plasma and liver lipids, and blood glucose levels of mice".《J Nutr Sci Vitaminol》.2008,第54卷第378-383页. * |
| QiShiSONG1 et al.."Tsaokoin |
| 李婷 等."加热回流法提取草果中抗氧化成分的研究".《食品研究与开发》.2009,第30卷(第8期),第23-26页. |
| 马洁 等."国产草果化学成分研究进展".《中国中医药信息杂志》.2005,第12卷(第9期),第97-98页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102552791A (en) | 2012-07-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6541582B2 (en) | Yuzu seed extract-containing composition, food for increasing skeletal muscle mass, and method for producing yuzu seed extract-containing composition | |
| CN103494292A (en) | Oily peony seed meal cake plant protein beverage and preparation method thereof | |
| CN105142424A (en) | Cereal containing hericium erinaceum and method for making same | |
| CN108947864A (en) | A kind of preparation method of ceramide | |
| CN104739726B (en) | A kind of Chinese medicine toothpaste and preparation method thereof | |
| KR100635025B1 (en) | A ginseng preparation using vinegar and process for thereof | |
| CN104544403A (en) | Beverage containing rose extract | |
| TW201340977A (en) | Des(rhamnosyl) acteoside-containing olive extract | |
| CN102552791B (en) | Active ingredient extracted from Amomum tsao-ko and application thereof in preparing blood sugar reducing medicine and food | |
| CN101167770A (en) | Laryngalgia anti-inflammation traditional Chinese medicinal preparation with improved taste and preparation method thereof | |
| CN101744986B (en) | Extraction method for ginseng, ophiopogon root and schisandra chinensis and preparation thereof | |
| CN103372081A (en) | Preparation method of Chinese herba preparation snake gall-dried orange peel oral liquid | |
| CN101744993B (en) | Extraction method for ginseng, ophiopogon root and schisandra chinensis and preparation thereof | |
| CN104435072B (en) | A kind of extract and preparation method thereof with auxiliary hyperglycemic, reducing blood lipid | |
| CN101744991B (en) | Single extraction method of ginseng, ophiopogon root and shiandra and preparation thereof | |
| CN107496510B (en) | Cyclocarya paliurus capsule and preparation method thereof | |
| CN101744996B (en) | Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof | |
| CN101744997B (en) | Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof | |
| CN101745016B (en) | Extraction method of 'ginseng/radix ophiopogonis and schisandra chinensis' and preparation thereof | |
| CN1081929C (en) | Health preparation of fresh Chinese angelica and its preparation | |
| CN101744994B (en) | Extraction method for ginseng, ophiopogon root and schisandra chinensis and preparation thereof | |
| CN106420932A (en) | Composition capable of increasing insulin sensitivity, and applications thereof | |
| CN101744987B (en) | Single extraction method of ginseng, ophiopogon root and shiandra and preparation thereof | |
| CN101744990B (en) | Method for individually extracting ginseng, radix ophiopogonis and schisandra chinensis and preparation thereof | |
| CN101745010B (en) | Extraction method of ginseng, ophiopogon root and shiandra and preparation thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140611 Termination date: 20150114 |
|
| EXPY | Termination of patent right or utility model |