CN103505498A - Preparation and application of effective part of total flavonoids in fenugreek - Google Patents
Preparation and application of effective part of total flavonoids in fenugreek Download PDFInfo
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- CN103505498A CN103505498A CN201210232186.4A CN201210232186A CN103505498A CN 103505498 A CN103505498 A CN 103505498A CN 201210232186 A CN201210232186 A CN 201210232186A CN 103505498 A CN103505498 A CN 103505498A
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Abstract
The invention discloses a preparation method and application of an effective part of total flavonoids in fenugreek. The method comprises the following steps: firstly adopting a diacolation extraction method in an extraction process; purifying an extracting solution by macroreticular resin after degreasing by ethyl acetate, so as to obtain the effective part of the total flavonoids in fenugreek, of which the content is more than 60%. A pharmacological experiment result shows that the effective part of the total flavonoids in the fenugreek has significant therapeutical effects on diseases in the aspects of diabetes mellitus and hyperlipidemia.
Description
Technical field
The present invention relates to Chinese medicine extraction and application, particularly a kind ofly from Semen Trigonellae, extract the method for total flavones and the application of total flavone valid target thereof.
Technical background
Semen Trigonellae is the seed of leguminous plant Trigonella Semen Trigonellae (Trigonella foenum-graecum L.), is a kind of traditional Chinese crude drug, by multi-section Chinese medicine ancient books and records, is included, and recording it has, and " gentle sun, by cold-damp." effect.Fenugreek seed is that a kind of Chinese herbal medicine is again that a kind of flavoring agent ， China, India, mediterranean country have plantation and application.Semen Trigonellae dry mature seed has been taken in the Pharmacopoeia of the People's Republic of China as conventional Chinese medicine.
The report of Semen Trigonellae is more, wherein relates to extraction and pharmacology's application of saponin, flavone.Chinese patent 200410070104.6 discloses a kind of from Semen Trigonellae extract, and it comprises polysaccharide, total flavones, three kinds of effective ingredient of saponin, has recorded in its extract general flavone content lower than 15% simultaneously.Chinese patent 200610066235.6 discloses a kind of Semen Trigonellae extract, has wherein recorded a kind of extracting method of total flavones, but the content of not mentioned total flavones.Chinese patent 200410029927.4 discloses a kind of method of extracting flavone from Semen Trigonellae, does not wherein record the content of flavone.Chinese patent 201110375609.3 discloses a kind of ultrasonic extraction of passing through, and macroporous resin separation and purification obtains the method for flavone, and its general flavone content is lower than 30%.
The general flavone content that extraction obtains from Semen Trigonellae of reporting in prior art document, all lower than 30%, does not reach the standard of Chinese medicine 5 classes.
Summary of the invention
In order to solve the shortcoming of prior art, the inventor proposes a kind of new method of extracting total flavones from Semen Trigonellae, comprises the following steps:
A, fenugreek seed is pulverized to No. two, rear mistake sieve according to a conventional method;
B, Semen Trigonellae coarse powder is extracted with alcohol-water solution percolation;
C, percolate is concentrated into without alcohol and obtains concentrated solution, the ethyl acetate extraction of its volume 1/2～1/5 1～3 time for concentrated solution, to remove wherein contained fat;
D, stripped concentrated solution are concentrated into without ethyl acetate, obtain liquid I;
E, liquid I are through macroporous resin (blade diameter length ratio 1: 9～1: 15) purification, and eluting order is:
The water elution of 2～5 column volumes;
The ethanol elution of 2～5 column volumes 20%～40%, collects ethanol elution, and concentrate drying obtains total flavones.
Another preferred version of the present invention is aqueous solution, the aqueous solution of ethanol, the mixing of one or more in the aqueous solution of the aqueous solution of propanol, isopropyl alcohol that the alcohol water described in step b is methanol, the aqueous solution of preferred alcohol.
The present invention is first extracted with ethyl acetate the liposoluble constituent in extracting solution, is conducive to subsequent purification, improves the content of total flavone valid target.
Another preferred version of the present invention is the preferred HPD600 type of macroporous resin macroporous resin used in step e.
Another preferred version of the present invention is the blade diameter length ratio described in step e preferably 1: 10.
Another preferred version of the present invention is aqueous solution, the aqueous solution of ethanol, one or more in the aqueous solution of the aqueous solution of propanol, isopropyl alcohol that 20%～40% alcohol water elution liquid described in step e is methanol, further preferred 25%～35% ethanol water.
Another preferred version of the present invention be as stated above in resulting extract general flavone content more than 60%.
The present invention also aims to provide a kind of medicine or food that contains the total flavones that extraction obtains from Semen Trigonellae.
The medicine that contains total flavones of the present invention has the effect for the treatment of diabetes.
The food that contains total flavones of the present invention is for improving diabetes patient's disease.
Semen Trigonellae extract of the present invention and pharmaceutically acceptable adjuvant routinely formulation method are made oral formulations, preferred tablet, capsule.
The mensuration of general flavone content in Semen Trigonellae extract, the Flavonoid substances in the middle of Semen Trigonellae is mainly flavonoid glycoside, take orientin as its labeled composition, by HPLC method, measures.
HPLC testing conditions: use C
18post is measured, mobile phase acetonitrile: isopropyl alcohol: water=8: 4: 88, mobile phase equaled 3.2 with phosphoric acid regulating ph value, and detection wavelength is 334nm, number of theoretical plate calculates and should be not less than 3000 by orientin.
The present invention has the following advantages: extraction process is simple, and extraction time is short, and purification by macroporous resin technique is simple, extracts the general flavone content obtain and be greater than 60% from Semen Trigonellae, meets the effective ingredient in Chinese standard of being used as medicine.
The specific embodiment
Embodiment 1
The preparation of Semen Trigonellae total flavone valid target of the present invention:
Take the Semen Trigonellae of 500 grams of pulverizing, cross sieve No. two, add in percolation bucket, with 60% alcohol dipping, percolation, percolation speed 3mL/min, collects 10L percolate, be concentrated into without alcohol and obtain concentrated solution, after ethyl acetate extracting twice with concentrated solution volume 1/2, concentrated solution is concentrated into without ethyl acetate, obtains liquid I.Liquid I is HPD600 macroporous resin (blade diameter length ratio 1: 9) above, uses successively the water of 4 column volumes, and 30% ethanol elution of 3 column volumes is collected the ethanol elution that merges 30%, and concentrated, the dry Semen Trigonellae extractive of general flavone that to obtain, contains total flavones 65%.
Embodiment 2
Take the Semen Trigonellae of 500 grams of pulverizing, cross sieve No. two, add in percolation bucket, with 60% alcohol dipping, percolation, percolation speed 3mL/min, collects 10L percolate, be concentrated into without alcohol and obtain concentrated solution, after ethyl acetate extraction once with concentrated solution volume 1/3, concentrated solution is concentrated into without ethyl acetate, obtains liquid I.Liquid I is HPD600 macroporous resin (blade diameter length ratio 1: 12) above, uses successively the water of 3 column volumes, and 40% ethanol elution of 2 column volumes is collected the ethanol elution that merges 40%, and concentrated, the dry Semen Trigonellae extractive of general flavone that to obtain, contains total flavones 70%.
Embodiment 3
Take the Semen Trigonellae of 500 grams of pulverizing, cross sieve No. two, add in percolation bucket, with 60% propanol dipping, percolation, percolation speed 3mL/min, collects 10L percolate, be concentrated into without alcohol and obtain concentrated solution, after ethyl acetate extracting twice with concentrated solution volume 1/5, concentrated solution is concentrated into without ethyl acetate, obtains liquid I.Liquid I is D201 macroporous resin (blade diameter length ratio 1: 15) above, uses successively the water of 4 column volumes, and 20% propanol eluting of 3 column volumes is collected the propanol eluent that merges 20%, and concentrated, the dry Semen Trigonellae extractive of general flavone that to obtain, contains total flavones 62%.
Embodiment 4
Take the Semen Trigonellae of 500 grams of pulverizing, cross sieve No. two, add in percolation bucket, with 60% alcohol dipping, percolation, percolation speed 3mL/min, collects 10L percolate, be concentrated into without alcohol and obtain concentrated solution, by the ethyl acetate of concentrated solution volume 1/4, extract after three times, concentrated solution is concentrated into without ethyl acetate, obtains liquid I.Liquid I is NKA-9 macroporous resin (blade diameter length ratio 1: 10) above, uses successively the water of 5 column volumes, and 30% ethanol elution of 5 column volumes is collected the ethanol elution that merges 30%, and concentrated, the dry Semen Trigonellae extractive of general flavone that to obtain, contains total flavones 68%.
Embodiment 5
Tablet preparation: from Semen Trigonellae, extract the extractive of general flavone 180g obtaining, hydroxypropyl emthylcellulose 160g, micropowder silica gel 58g, magnesium stearate 2g, mix homogeneously, crosses 80 mesh sieves, and dry pressing is granulated, with 20 mesh sieve granulate, tabletting.
Embodiment 6
Capsule preparation: the extractive of general flavone 200g extracting in Semen Trigonellae, add pregelatinized Starch 80g, using 95% ethanol as adhesive, cross 20 mesh sieve soft material processed, 60 ℃ dry, granulate, dry granule added the crosslinked CMC-Na12g of 100 objects and micropowder silica gel 3g to mix, measure the content of index composition in granule, encapsulated, make capsule.
Embodiment 7
The hypoglycemic activity research experiment of Semen Trigonellae total flavone valid target to diabetes rat:
Select the Wistar healthy rat of body weight 170～200g, male and female half and half.Experimental group rat single intraperitoneal injection streptozotocin 50mg/kg (is dissolved in 0.1mol/L citrate buffer solution, pH=4.2) prepares diabetes model.Injection streptozotocin detects blood glucose and glucose in urine after 3 days.Glucose in urine >=3+, blood glucose >=16.7mmol/L lists diabetes study object in.Matched group is the above-mentioned buffer of lumbar injection equal-volume simultaneously.
Experimental technique one: by becoming the diabetes rat of mould to be divided at random the high, medium and low dosage group of diabetic groups, positive controls and Semen Trigonellae extract, separately establish Normal group.The high, medium and low dosage treatment group of Semen Trigonellae extract gavage gives Semen Trigonellae extract 1.5mL/100g body weight (being equivalent to respectively Semen Trigonellae extract 400mg/kg, 200mg/kg, 100mg/kg body weight).Positive control drug lotensin gavage gives 15mg/kg body weight (1.5mL/100g body weight), and contrast combination diabetic groups only gavage gives 1.5mL/100g body weight drinking water.Every day, gavage was 1 time, totally 12 weeks.
Experimental technique two: by becoming the diabetes rat of mould to be divided at random diabetic groups and Semen Trigonellae extracting solution treatment group, separately establish Normal group.Semen Trigonellae extracting solution treatment group gavage gives Semen Trigonellae extracting solution 1.5mL/100g body weight (being equivalent to Semen Trigonellae extract 400mg/kg body weight).Matched group and diabetic groups only gavage give 1.5mL/100g body weight drinking water.Experiment totally 6 weeks.
Statistical procedures: data result represents with X ± S, relatively adopts variance analysis between group.
1. the time-effect relationship that Semen Trigonellae extract affects blood glucose in diabetic rats
Press experimental technique one, within the 3rd week, 4 weeks, 6 weeks, 8 weeks and 12 weeks before administration and after administration, respectively detect blood sugar content, the results are shown in Table 1.
The time-effect relationship of table 1 Semen Trigonellae extract on blood glucose in diabetic rats impact
With diabetic groups comparison,
*p < 0.05,
*p < 0.01; With matched group comparison,
△p < 0.05,
△ △p < 0.01
Interpretation of result: Semen Trigonellae extract can significantly reduce blood glucose in diabetic rats content.After medication, blood sugar content significantly reduces by 3 weeks time, is down to matched group without marked difference, and continues 12 weeks in the time of 4 weeks.
Press experimental technique two, administration in first 4 weeks, every day, gavage was 1 time, drug withdrawal in latter 2 weeks, totally 6 weeks.In the 1st week, 3 weeks, 4 weeks, 5 weeks and 6 weeks, respectively check blood glucose and glucose in urine content, the results are shown in Table 2.
The time-effect relationship of table 2 Semen Trigonellae extract on blood glucose in diabetic rats impact
With diabetic groups comparison,
*p < 0.05,
*p < 0.01; With matched group comparison,
△p < 0.05,
△ △p < 0.01
Interpretation of result: Semen Trigonellae extract can significantly reduce blood glucose in diabetic rats content.After medication, blood sugar content significantly reduces by 3 weeks time; And drug withdrawal 2 weeks, blood glucose gos up slower, and blood glucose continues significantly longer lower than the time of diabetes rat.
2. Semen Trigonellae extract is tested diabetes rat glucose-tolerant
Press experimental technique two, do glucose-tolerant experiment 4 weekends, rat gives within 30 minutes, 60 minutes, 90 minutes and 120 minutes, to measure blood sugar content after glucose, the results are shown in Table 3.
The result of table 3 Semen Trigonellae extract administration to diabetes rat glucose tolerance test
With diabetic groups comparison,
*p < 0.05,
*p < 0.01; With matched group comparison,
△p < 0.05,
△ △p < 0.01
Interpretation of result: Semen Trigonellae extract can improve the glucose tolerance of diabetes rat.
In sum: Semen Trigonellae extract can obviously reduce diabetes rat blood sugar level, improve the glucose tolerance of diabetes rat.After medication, blood sugar content obviously reduces by 3 weeks time; And drug withdrawal is after 2 weeks, blood glucose gos up slower, and blood glucose continues in the reduced levels time longer.
Above-described embodiment is only the preferred embodiments of the present invention; be not limited to the present invention; for a person skilled in the art; in the situation that not paying creative work; all any changes of doing within the spirit and principles in the present invention, within being all included in protection scope of the present invention.
Claims (10)
1. from fenugreek seed, extract a method for total flavone valid target, it is characterized in that extraction comprises the following steps:
A, fenugreek seed is pulverized to No. two, rear mistake sieve according to a conventional method;
B, Semen Trigonellae coarse powder is extracted with alcohol-water solution percolation;
C, percolate is concentrated into without alcohol and obtains concentrated solution, the ethyl acetate extraction of its volume 1/2～1/5 1～3 time for concentrated solution;
D, stripped concentrated solution are concentrated into without ethyl acetate, obtain liquid I;
E, liquid I are through macroporous resin (blade diameter length ratio 1: 9～1: 15) purification, and eluting order is:
The water elution of 2～5 column volumes;
The alcohol water elution of 2～5 column volumes 20%～40%, collects alcohol water elution liquid, and concentrate drying obtains Semen Trigonellae extract, and wherein general flavone content is more than 60%.
2. according to described in e step in claim 1, it is characterized in that preferred HPD600 macroporous resin.
3. according to described in e step in claim 1, be further characterized in that preferably 3～4 column volume water elutions.
4. according to described in e step in claim 1, be further characterized in that the preferably alcohol water elution of 3～4 column volumes 20%～40%.
5. according to claim 4, it is characterized in that alcohol water concentration preferably 25%～35%.
6. according to described in the e step in claim 1, it is characterized in that alcohol water be the aqueous solution of methanol, the aqueous solution of the aqueous solution of ethanol, propanol, the mixing of one or more in the aqueous solution of isopropyl alcohol, the aqueous solution of preferred alcohol.
7. method according to claim 1, is characterized in that the total flavones obtaining is for the preparation of the medicine for the treatment of diabetes, hyperlipidemia.
8. method according to claim 1, is characterized in that the total flavones obtaining is for the preparation of the food that improves diabetes, hyperlipidemia.
9. according to described in claim 1 or 7, it is characterized in that extracting the total flavones and the pharmaceutically acceptable adjuvant that obtain and make oral formulations according to conventional formulation method from fenugreek seed.
10. according to claim 9, it is characterized in that oral formulations preferred tablet, capsule.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114288331A (en) * | 2021-10-29 | 2022-04-08 | 中国医学科学院药用植物研究所 | Method for simultaneously extracting volatile oil from effective parts of total flavonoids and total saponins of Chinese medicinal fenugreek, extract and application thereof |
| CN115645466A (en) * | 2022-09-23 | 2023-01-31 | 烟台新时代健康产业有限公司 | Anti-fatigue traditional Chinese medicine effective part composition and preparation method and application thereof |
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| CN1605357A (en) * | 2004-07-30 | 2005-04-13 | 北京星昊现代医药有限公司 | Fenugreek seed extract and its preparing process and application |
| CN102441026A (en) * | 2011-11-22 | 2012-05-09 | 中国科学院西北高原生物研究所 | Fenugreek flavonoids extract preparation method and blood sugar level decreasing application thereof |
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| CN1605357A (en) * | 2004-07-30 | 2005-04-13 | 北京星昊现代医药有限公司 | Fenugreek seed extract and its preparing process and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114288331A (en) * | 2021-10-29 | 2022-04-08 | 中国医学科学院药用植物研究所 | Method for simultaneously extracting volatile oil from effective parts of total flavonoids and total saponins of Chinese medicinal fenugreek, extract and application thereof |
| CN115645466A (en) * | 2022-09-23 | 2023-01-31 | 烟台新时代健康产业有限公司 | Anti-fatigue traditional Chinese medicine effective part composition and preparation method and application thereof |
| CN115645466B (en) * | 2022-09-23 | 2023-11-21 | 烟台新时代健康产业有限公司 | Anti-fatigue traditional Chinese medicine effective part composition and preparation method and application thereof |
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Application publication date: 20140115 |