CN103446198B - Tibetan medicine Primula sikkimensis antioxidant extract and its production and use - Google Patents
Tibetan medicine Primula sikkimensis antioxidant extract and its production and use Download PDFInfo
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- CN103446198B CN103446198B CN201310415409.5A CN201310415409A CN103446198B CN 103446198 B CN103446198 B CN 103446198B CN 201310415409 A CN201310415409 A CN 201310415409A CN 103446198 B CN103446198 B CN 103446198B
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Abstract
The present invention relates to the Primula sikkimensis effective extract and preparation method thereof containing Wheat Protein, described effective extract is selected from one of the ligroin extraction, chloroform extract, ethyl acetate extract, n-butanol extract and combination thereof that to extract from Primula sikkimensis ethanol extract and obtain, research proves, wherein ligroin extraction, chloroform extract, ethyl acetate extract, n-butanol extract have obvious external removing hydroxyl radical free radical ability; Ethyl acetate extract and n-butanol extract have obvious external removing DPPH(hexichol for bitterness hydrazine) ability of fat free love base, therefore, described effective extract can be used for preparing anti-oxidation medicine and cosmetics.
Description
Technical field
The present invention relates to a kind of Tibetan medicine Primula sikkimensis antioxidant extract and preparation method thereof; The invention further relates to the drug regimen of described extract; The invention still further relates to the application of described extract in anti-oxidation medicine or cosmetics; Belong to the field of Chinese medicines.
Background technology
1956, British Harman proposed " free radical theory ", and this theory thinks that free radical is attacked life macromolecule and caused tissue injury, and being the basic reason causing body aging, is also the great reason of induced tumor malignant disease.That studies free radical along with people gos deep into, and this theory is also that increasing people accepts.Free radical refers to " any atom or atomic group comprising a unpaired electron ", very big to Health Impact.Under physiological conditions, oxygen is in reduced levels, and it produces and removing is in dynamic equilibrium, but under some pathologic condition, free radical is superfluous, causes body injury.Free radical is except itself has damage biomacromolecule (protein, DNA), also can cause the lipid peroxidation (LPO) of polyunsaturated fatty acid, and the end-product of LPO reaction is malonaldehyde (MDA), thus makes protein, nucleic acid, cephalin occur to be cross-linked and lose its activity.Large quantity research shows, the sudden change of disease that ageing-related and gene, the damage all caused with free radical as cancer, cardiovascular disease, rheumatic arthritis, diabetes, nervous system disease, aging etc. is correlated with, and removes free radical unnecessary in body and just can prevent senescence and disease.Therefore seek to utilize human body to be easy to absorb, a new study hotspot can be become by the Exogenous Antioxidants of excessive free radicals in purged body.But, the genotoxic potential become increasingly conspicuous along with synthetized oxidation preventive agent and carcinogenesis are repelled by people, from plant, find the inexorable trend that antioxidant that is natural, efficient, low toxicity just becomes the development of current antioxidant, specify direction simultaneously also for modern medicine and healthcare industry.
Primulaceae (
primulaceae) belong to the section of Dicotyledoneae Dilleniidae, perennial or annual herb, about 22 belong to 800 kinds, and blazon the whole world, main product is in temperate zone, the Northern Hemisphere; In domestic 12 belong to about 500 kinds, there is distribution all parts of the country.This section's floristics is many, and pharmacological action is extensive, mainly contains the serum uric acid level reducing mice, promote rat bile secretion, reduce the gallstone formation rate of bile pigment calculus, the functions such as immunomodulating, it is reported that its main chemical compositions has flavonoid, terpenoid, sterols, organic acid, quinones etc.Primula sikkimensis (
primula Sikkimensdishook), having another name called Primula sikkmensis Hook., belong to Primulaceae primula, is a kind of common Tibetan medicine material, is used as medicine with flower, is that former plant " protected " by Tibetan medicine as will color.Brightly yellowish color, mitriform, consor in scape top, main product in Eastern Tibet and south, southeast Qinghai, western Sichuan, northwestern Yunnan Province; Be mainly used in heat-clearing and toxic substances removing, the diseases such as heart arteries and veins stasis blocking, blood vessels are not smooth, the clinician through several Tibetan medicine hospital facts have proved, in treatment heart arteries and veins stasis blocking, blood vessels are smooth, determined curative effect, in Ganzizangzu area, Tibetan also widely use, and through resource investigation, resource is very abundant.Its chemical composition has no report, not seen in the report of Primula sikkimensis and effective site Study on antioxidation and application aspect.We have carried out the preliminary study of antioxidant activity to its total extract and different solvents polar fraction, and activity experiment shows: its total extract and some polar fraction have good antioxidant activity.
Summary of the invention
An object of the present invention is, provides antioxidant extract of a kind of Primula sikkimensis and preparation method thereof.Two of object of the present invention is, provides a kind of pharmaceutical composition being effective ingredient with described extract.Three of object of the present invention is, provides described extract preparing the application in antioxidation and related drugs thereof and cosmetics.
The present invention compares the antioxidant activity of the extract of different solvents, determines extract with antioxidation and preparation method thereof.
Primula sikkimensis extract of the present invention be selected to extract from Primula sikkimensis ethanol extract obtain ligroin extraction (XJ-1), chloroform extract (XJ-2), ethyl acetate extract (XJ-3), n-butanol extract (XJ-4) and water extract (XJ-5) one or a combination set of; Preferably extract from Primula sikkimensis ethanol extract obtain ligroin extraction (XJ-1), chloroform extract (XJ-2), n-butanol extract (XJ-4) or its combination; Or preferably extract from Primula sikkimensis ethanol extract obtain ethyl acetate extract (XJ-3), n-butanol extract (XJ-4) or its combination.
Extract of the present invention can through extracting, concentrated, series extraction obtains, its preparation method comprises the following steps:
(1) get Primula sikkimensis herb coarse powder, by soak with ethanol, ultrasound wave hydrotropy extracts, and filters, and filtering residue repeats said extracted, filters, merge extractive liquid;
(2) extracting solution concentrating under reduced pressure is obtained concentrated solution, then concentrated solution is mixed with water, obtain the concentrated solution after diluting.
(3), with opposed polarity solvent petroleum ether, chloroform, ethyl acetate, the extraction of n-butyl alcohol gradient, often kind of solvent repeats
Extraction, merge identical organic facies, concentrating under reduced pressure obtains the extract of each solvent.
Described method preferably includes following steps: (1) get Primula sikkimensis herb coarse powder, soak 24 h by the different concentration ethanol of 30 times of quality, ultrasound wave hydrotropy extracts 1 h, filter, filtering residue repeats said extracted process 2 times, filters, merge three extracting solution, wherein the preferred 60-90% ethanol of ethanol used.(2) extracting solution being evaporated to relative density is 1.10-1.24 mg/mL (55 DEG C), obtains concentrated solution, then by concentrated solution and water by volume 1:1 mix, obtain the concentrated solution after diluting; (3) extract with the rear concentrated solution isopyknic opposed polarity solvent petroleum ether of dilution, chloroform, ethyl acetate, n-butyl alcohol gradient, re-extract 2 times distinguished by often kind of solvent, and merge identical organic facies, concentrating under reduced pressure obtains the extract of each solvent.
The present invention also provides the pharmaceutical composition of each solvent extractable matter prepared in this way.Described pharmaceutical composition is for effective ingredient with extract of the present invention, formed with pharmaceutically acceptable carrier, and exist with suitable pharmaceutical dosage form, these preparations can be tablet (preferred sugar coated tablets, film coated tablet, enteric coated tablet, slow releasing tablet), capsule (preferred hard capsule, soft capsule, slow releasing capsule), oral liquid, mixture, suck agent, granule, electuary, pill, powder, unguentum, sublimed preparation, suspensoid, solution, injection, injectable powder, lyophilized injectable powder, suppository, ointment, plaster, cream, spray, drop pill, drop pill, patch etc.
Invention further provides various extract preparation treatment and or prevention oxidative drug and cosmetics in application.The antioxidation related experiment of for this reason carrying out is to remove DPPH free radical, hydroxyl radical free radical for activity index.Experimental result shows, ethyl acetate extract and n-butanol extract have the ability of obvious external removing DPPH fat free love base; Ligroin extraction, chloroform extract and n-butanol extract have better removes hydroxyl radical free radical, has antioxidation, can be used for preparing anti-oxidation medicine and cosmetics.
specific embodiments:
embodiment 1:
The preparation method of each extract:
1) total extract extracts
Get Primula sikkimensis herb coarse powder 20 g, with 600 ml 90% soak with ethanol 24 h, ultrasound wave hydrotropy extracts 1 h, filters, and filtering residue repeats said extracted process 2 times, filters, merges three extracting solution.
2) concentrated
Extracting solution decompression recycling ethanol is obtained concentrated solution (relative density is 1.15g/mL, 55 DEG C), then by concentrated solution and water by volume 1:1 mix, obtain the concentrated solution (90 ml) after diluting.
3) gradient extraction
Use petroleum ether (90 ml/ time × 3 times) successively, chloroform (90 ml/ time × 3 times), ethyl acetate (90 ml/ time × 3 times), concentrated solution after n-butyl alcohol (90 ml/ time × 3 times) extraction dilution, merge identical organic facies, concentrating under reduced pressure, obtain ligroin extraction (XJ-1, 0.33 g, extraction ratio: 1.65%), chloroform extract (XJ-2, 0.16 g, extraction ratio: 0.8%), ethyl acetate extract (XJ-3, 0.38 g, extraction ratio: 1.9%), n-butanol extract (XJ-4, 0.07 g, 0.35%) and water extract (XJ-5 extraction ratio:, 0.8 g, extraction ratio: 4%).
embodiment 2:
The preparation method of each extract:
1) total extract extracts
Get Primula sikkimensis herb coarse powder 30 g, with 900 ml 65% soak with ethanol 24 h, ultrasound wave hydrotropy extracts 1 h, filters, and filtering residue repeats said extracted process 2 times, filters, merges three extracting solution.
2) concentrated
Extracting solution decompression recycling ethanol is obtained concentrated solution (relative density is 1.10g/ml, 55 DEG C), then by concentrated solution and water by volume 1:1 mix, obtain the concentrated solution (100 ml) after diluting.
3) gradient extraction
Use petroleum ether (100 ml/ time × 3 times) successively, chloroform (100 ml/ time × 3 times), ethyl acetate (100 ml/ time × 3 times), concentrated solution after n-butyl alcohol (100 ml/ time × 3 times) extraction dilution, merge identical organic facies, concentrating under reduced pressure, obtain ligroin extraction (XJ-1, 0.36 g, extraction ratio: 1.20%), chloroform extract (XJ-2, 0.05 g, extraction ratio: 0.17%), ethyl acetate extract (XJ-3, 0.07 g, extraction ratio: 0.23%), n-butanol extract (XJ-4, 0.27 g, 0.90%) and water extract (XJ-5 extraction ratio:, 1.2 g, extraction ratio: 4.0%).
embodiment 3:
Free radical scavenging is tested:
Prepared each polar fraction in embodiment 1 is adopted to carry out activity experiment.
Antioxidant activity represents with scavenging ability of DPPH free radical size.According to the experiment condition that preliminary experiment is determined, measure the activity that fat free love base DPPH removed by the different sample of Primula sikkimensis.Get variable concentrations sample solution 2.0 mL, add 2.0 mL 1.52 × 10
-4the DPPH ethanol solution of mmol/L fully mixes, and room temperature lucifuge take solvent as blank after leaving standstill 30 min, and 517 nm places survey absorbance A
1; Replace sample solution to do negative control with same volume solvent, measure absorbance A
2; Replace DPPH solution to do blank group with same volume dehydrated alcohol, measure absorbance A
3.Take VC as contrast, often group does 3 repetitions, asks its meansigma methods.Be calculated as follows clearance rate:
Sample is to clearance rate (%)=[1-(A of DPPH
1-A
3)/A
2] × 100%
embodiment 4:
Remove hydroxyl radical free radical activity test:
Prepared each polar fraction in embodiment 1 is adopted to carry out activity experiment.
Antioxidant activity represents to remove hydroxyl radical free radical capacity of water.According to the experiment condition that preliminary experiment is determined, measure the activity that hydroxyl radical free radical removed by the different sample of Primula sikkimensis.By 1.5 mL 1.8 mol/L salicylic acid solutions and 2.0 mL 1.8 mol/L FeSO
4after solution mixes in test tube, add 1 mL variable concentrations sample solution, then add 0.1 mL 0.03% H
2o
2, shake up, in 37 DEG C of insulation 30 min, 510 nm places record sample sets absorbance A
i; Simultaneously by H in sample sets
2o
2change 0.1 mL distilled water into, record sample reference group absorbance A
j; Sample in sample sets is changed into 1.0 mL solvents, record blank group absorbance A
0.Take VC as contrast, often group does 3 repetitions, asks its meansigma methods.Be calculated as follows clearance rate:
OH clearance rate (%)=[A
0-(A
i-A
j)]/A
0× 100%
The external free radical scavenging experiment in each position of table 1 Primula sikkimensis
Note: IC
50± s, n=3
The each position of table 2 Primula sikkimensis external removing hydroxyl radical free radical activity experiment
Result shows; the ligroin extraction (XJ-1) adopting present invention process to prepare, chloroform extract (XJ-2), ethyl acetate extract (XJ-3), n-butanol extract (XJ-4) have good antioxidant activity; wherein ligroin extraction, chloroform extract, n-butanol extract have good removing hydroxyl radical free radical ability, and resistance to oxidation is about 5/6,1/4,3/4 of VC respectively; Ethyl acetate extract and n-butanol extract have good scavenging ability of DPPH free radical, and resistance to oxidation is respectively 1/11 and 1/7 of VC; Wherein ligroin extraction, chloroform extract, ethyl acetate extract, n-butanol extract are removed hydroxyl radical free radical ability and are better than VC in concentration lower than during 167 μ g/mL.
Claims (6)
1. the activity extract of Primula sikkimensis is preparing the application in antioxidative medicine or cosmetics, it is characterized in that described activity extract is selected from Primula sikkimensis ethanol extract the ligroin extraction (XJ-1), n-butanol extract (XJ-4) one or a combination set of that extract and obtain; Described activity extract adopts the method comprising following steps to prepare: (1) get Primula sikkimensis herb coarse powder, and by soak with ethanol, ultrasound wave hydrotropy extracts, and filters, and filtering residue repeats said extracted, filters, merge extractive liquid; (2) extracting solution concentrating under reduced pressure is obtained concentrated solution, then concentrated solution is mixed with water, obtain the concentrated solution after diluting; (3) carry out gradient extraction with opposed polarity solvent petroleum ether, chloroform, ethyl acetate, n-butyl alcohol, often kind of solvent re-extract, merges identical organic facies, and namely concentrating under reduced pressure obtains the extract of each solvent.
2. application according to claim 1; it is characterized in that: described method preferably includes following steps: (1) gets Primula sikkimensis herb; 24 h are soaked by the different concentration ethanol of 30 times of quality; ultrasound wave hydrotropy extracts 1 h; filter; filtering residue repeats said extracted process 2 times, filters, merges three extracting solution; (2) extracting solution being evaporated to the relative density recorded at 55 DEG C is 1.10-1.24, obtains concentrated solution, then by concentrated solution and water by volume 1:1 mix, obtain the concentrated solution after diluting; (3) extract with the rear concentrated solution isopyknic opposed polarity solvent petroleum ether of dilution, chloroform, ethyl acetate, n-butyl alcohol gradient, re-extract 2 times distinguished by often kind of solvent, and merge identical organic facies, concentrating under reduced pressure obtains the extract of each solvent.
3. an application according to claim 2, is characterized in that: the preferred 60-90% ethanol of described ethanol.
4. the application according to any one of claim 1-3, is characterized in that, described activity extract is made pharmaceutical composition as effective ingredient and pharmaceutically acceptable carrier.
5. application according to claim 4, it is characterized in that, the dosage form of described pharmaceutical composition can be tablet, capsule, oral liquid, suck agent, granule, pill, powder, unguentum, sublimed preparation, suspensoid, solution, injection, suppository, cream, spray, drop pill, patch.
6. application according to claim 5, is characterized in that described tablet is selected from sugar coated tablet, film coated tablet, enteric coated tablet or slow releasing tablet; Described capsule is selected from hard capsule, soft capsule or slow releasing capsule.
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