CN101716197B - Extractive of Taxus chinensis var.mairei leaves and preparation method - Google Patents
Extractive of Taxus chinensis var.mairei leaves and preparation method Download PDFInfo
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- CN101716197B CN101716197B CN2009101570340A CN200910157034A CN101716197B CN 101716197 B CN101716197 B CN 101716197B CN 2009101570340 A CN2009101570340 A CN 2009101570340A CN 200910157034 A CN200910157034 A CN 200910157034A CN 101716197 B CN101716197 B CN 101716197B
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- 241000508252 Taxus mairei Species 0.000 title claims abstract description 22
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- 238000000605 extraction Methods 0.000 claims abstract description 34
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- 229960001285 quercetin Drugs 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extractive of Taxus chinensis var.mairei leaves and a preparation method. The extractive is a straw yellow powder. The powder contains sciadopitysin the weight content of which is 65-70 percent; the sciadopitysin contains the following five components: 3-O-rutin-quercetol, 3-O-rutin-campherol, 3-O-rutin-myricetin, 7-O-glucose-campherol and 7-O-glucose-quercetol, and the total weight content of the five components in the sciadopitysin is 40-60 percent. The extractive is prepared by the preparation method comprising the steps of baking, crushing and screening, immersing into an alcohol dissolvant, ultrasonically extracting while stirring, decompressing and concentrating an extracting solution to remove alcohol, extracting with chloroform and degreasing, water phase concentrating and drying by taking fresh Taxus chinensis var.mairei leaves as raw materials. The extractive of Taxus chinensis var.mairei leaves has the functions of improving heat microcirculation, resisting arrhythmia, lowering myocardial oxygen consumption and the like and having the therapeutic and health-care function on diseases of cardiovascular system; and the preparation method has low energy consumption, short extracting time, few impurities and higher extraction efficiency.
Description
Technical field
The present invention relates to effective ingredients in plant and extractive technique, be specifically related to a kind of extract and method for preparing of Taxus mairei blade.
Background technology
From Taxus (genus Taxus) plant, separating the paclitaxel that obtains is first kind of effective natural anti-cancer drugs, and paclitaxel has been widely used in the clinical treatment of all kinds of tumors, and receives the attention of countries in the world more and more.Except that containing paclitaxel, also contain one type and have the active material of valuable pharmacological: the Ramulus et folium taxi cuspidatae flavone in the Ramulus et folium taxi cuspidatae medication composition.Flavone compound (Flavonoids) claims that again bioflavonoids (bioflavonoids) is one a type low molecule Secondary Metabolism of Plant thing, is distributed widely in vegetable, fruit and the medicinal plants.This compounds has common parent nucleus C
6-C
3-C
6Structure from vegetable material, separated having obtained hundreds of kind flavone compound at present, and new chemical compound is coming to light constantly also.Different according to substituent group and position thereof, can it be divided into I aglycon-apigenin (Apigenin) and be main body, V naringenin (Naringin) flavanone glycoside (Bi-hydroflavonoids) chemical compound for main body, III aglycon-kaempferol (Kaempferol) for main body, IV aglycon-Quercetin (Quercetin) for main body etc. for main body, II aglycon-luteolin (Luteolin):
The main pharmacotoxicological effect of Flavonoid substances is: to cardiovascular effect, antiinflammatory and anti-immunization, anti-microbial effect, to the effect and the antitumor action of peptic ulcer.Antitumor action discovers that flavone compound is through promoting tumor necrosis factor, suppressing number of ways performance curative effects such as carcinogen and antioxidation.The Ramulus et folium taxi cuspidatae flavone and the method for distilling that from Ramulus et folium taxi cuspidatae, extract are not at present also seen patent and bibliographical information.
The effective ingredients in plant extractive technique has nearly 5000 history, and traditional extraction process can be divided into two big types according to leaching process to the difference of energy requirement mode.One type is heating extraction, mainly contains different modes such as decocting extraction method, reflux extraction and soxhlet extraction; Another kind of is the soaking and extracting method, mainly contains two kinds of dipping extraction method and percolation extraction methods.Traditional extraction process exist extraction time long, technology is complicated, efficient is low, industrial pollution is big and target compound extracted defective such as non-selectivity.Use the important core technology means of ultrasonic-assisted extraction effective ingredients in plant in recent years, the ultrasonic-assisted extraction technology is to utilize supersonic vibration to increase the permeability that solvent gets into plant cell, strengthens the mass transfer rate of extract between two-phase medium.Ultrasonic vibration can also produce cavitation bubble, and bubble strenuous exercise pair cell forms powerful shearing force, forms local assault ripple and high-speed jet effect when particularly bubble collapses, and plant cell is broken, and quickens the release of cellular content; Ultrasonic extraction can carry out in lower temperature range, also can effectively prevent purpose composition degraded in the plant, and extract is had high selectivity, and extraction time is short, and extract purity and extraction yield are all higher.
Summary of the invention
Technical problem to be solved by this invention provides a kind of heart of improvement microcirculation that has, and arrhythmia reduces myocardium keto consumption etc., to the extract of the Taxus mairei blade of the treatment of cardiovascular system diseases and health-care effect.
The present invention also provides this preparation method of extract.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of extract of Taxus mairei blade; This extract is a pale yellow powder; Contain weight content in this powder and be 65～70% Ramulus et folium taxi cuspidatae flavone; Said Ramulus et folium taxi cuspidatae flavone comprises following 5 kinds of compositions: 3-O-rutin-Quercetin, 3-O-rutin-kaempferol, 3-O-rutin-myricetin, 7-O-glucose-kaempferol and 7-O-glucose-Quercetin; The gross weight content of above-mentioned 5 kinds of compositions is 40～60% in the said Ramulus et folium taxi cuspidatae flavone; This extract is a raw material with fresh southern Semen Phaseoli blade, and supersound extraction, extracting solution concentrating under reduced pressure go alcohol, chloroform extraction defat, water concentrate drying step to make down through oven dry, crushing screening, immersion alcohol solvent, stirring.
Ramulus et folium taxi cuspidatae flavones content detection method is according to Al
3+-rutin binary complex fluorophotometric method is analyzed, excitation spectrum bandwidth 3nm, excitation wavelength lambda
Ex436nm, emission spectra bandwidth 5nm, λ
Em483nm, rutin standard solution fluorescence intensity to the respective concentration mapping quantitatively.
The assay method of the total content of 3-O-rutin-Quercetin, 3-O-rutin-kaempferol, 3-O-rutin-myricetin, 7-O-glucose-kaempferol and 5 kinds of compositions of 7-O-glucose-Quercetin adopts high-efficient liquid phase chromatogram technique analysis; Chromatographic column is Varian; Microsorb-MV100C18; Detect wavelength 360nm, mobile phase is methanol=55: 45, and phosphoric acid is transferred pH=2.5; Column temperature is 25 ℃, and flow velocity is 1.0ml/min, and sample size is 10 μ l, and the standard substance external standard method is quantitative.
This extract is effective composition of medicine for cardiovascular system or health food; The active ingredient of granule, tablet, capsule, drop pill, soft capsule or the injection of medicine for cardiovascular system can be thought, also the active ingredient of cardiovascular system health food can be.
A kind of preparation method of extract of Taxus mairei blade comprises the steps:
1,, be to dry 20～30 hours under 55～65 ℃ of conditions in temperature with fresh Taxus mairei blade;
2, with the Taxus mairei blade of above-mentioned oven dry be ground into can through 0.45 μ m sieve for extracting material, weigh;
3, the said extracted material is packed in the ultrasonic extraction still, add concentration again and be 40～60% ethanol, extracting material and alcoholic acid w/v (Kg/L) is 1: 15～17;
4, be under 35～55 ℃ of conditions then in temperature; Use ultrasonic sounding of independent-excited and radial vibration column transducer supersound extraction 20～30 minutes while stirring; The supersound extraction mode be each ultrasonic 3 minutes with at interval 2 minutes once ultrasonic; Ultrasonic power is 100W, and supersonic frequency is 30-70kHz, and supersound extraction is accomplished after-filtration and obtained extracting solution; Ultrasonic sounding of independent-excited and radial vibration column transducer are prior art, and its structure and operation principle are not introduced at this;
5, go pure phase at said extracted liquid elder generation concentrating under reduced pressure, the solution after will going alcohol mutually again is with the chloroform extraction defat of 3 times of volumes, and the defat water concentrate drying that finishes obtains containing the extract of the Taxus mairei blade of Ramulus et folium taxi cuspidatae flavone.It all is this area routine techniques that concentrating under reduced pressure removes alcohol, chloroform extraction defat, concentrate drying, does not detail at this.
Compared with prior art; The invention has the advantages that a kind of extract of Taxus mairei blade; This extract is a pale yellow powder; Contain weight content in this powder and be 65～70% Ramulus et folium taxi cuspidatae flavone; The Ramulus et folium taxi cuspidatae flavone comprises following 5 kinds of compositions: 3-O-rutin-Quercetin, 3-O-rutin-kaempferol, 3-O-rutin-myricetin, 7-O-glucose-kaempferol and 7-O-glucose-Quercetin; The gross weight content of above-mentioned 5 kinds of compositions is 40～60% in the Ramulus et folium taxi cuspidatae flavone, and this extract is a raw material with fresh southern Semen Phaseoli blade, and supersound extraction, extracting solution concentrating under reduced pressure go alcohol, chloroform extraction defat, water concentrate drying step to make down through oven dry, crushing screening, immersion alcohol solvent, stirring; This extract can antiplatelet aggregation and the outer thrombosis of antibody; There is blood circulation promoting and blood stasis dispelling to improve the microcirculatory effect of heart, arrhythmia is also arranged, reduce the effect of myocardium keto consumption; Simultaneously can decreased heart rate, bring high blood pressure down, reduce effect such as coronary resistance, help anginal alleviation.Therefore the present invention is a kind of heart of improvement microcirculation that has, and arrhythmia reduces myocardium keto consumption etc., to the extract of the Taxus mairei blade of the treatment of cardiovascular system diseases and health-care effect.Method for preparing of the present invention has the high temperature of need not, and energy consumption is low, and extraction time is short, and impurity is few, extraction ratio advantage of higher, the extraction rate reached to 98.76% of Ramulus et folium taxi cuspidatae flavone in the blade.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment
With fresh Taxus mairei blade 50kg,, pulverize through 55～65 ℃ of oven dry 20～30h; Cross 0.45 μ m sieve, in the ultrasonic extraction still of packing into, add 40～60% ethanol, 750～850L; Mix, under 35～55 ℃ of temperature conditions, the limit gas-lifting type stirs the limit with the ultrasonic sounding of independent-excited and radial vibration column transducer supersound extraction 20～30min; Ultrasonic power is 100W, and supersonic frequency is 33kHz, and the supersound extraction mode is each ultrasonic 3min; Every interval 2min is once ultrasonic, and warp is 4～6 supersound extraction after-filtration altogether, obtain extracting solution; Extracting solution elder generation concentrating under reduced pressure removes alcohol; To go the chloroform extraction defat of the solution of alcohol after mutually with 3 times of volumes again, the defat after drying obtains containing the extract of the Taxus mairei blade of Ramulus et folium taxi cuspidatae flavone, contains weight content in this extract and be 65～70% Ramulus et folium taxi cuspidatae flavone; Comprise following 5 kinds of compositions in the Ramulus et folium taxi cuspidatae flavone: 3-O-rutin-Quercetin, 3-O-rutin-kaempferol, 3-O-rutin-myricetin, 7-O-glucose-kaempferol and 7-O-glucose-Quercetin, the gross weight content of above-mentioned 5 kinds of compositions is 40～60% in the Ramulus et folium taxi cuspidatae flavone.The Ramulus et folium taxi cuspidatae flavones content adopts Al
3+The analysis of-rutin binary complex fluorophotometric method records.The total content of 5 kinds of compositions adopts high effective liquid chromatography for measuring.Among this embodiment in the southern Taxus leaf sheet Ramulus et folium taxi cuspidatae flavone extraction ratio can reach 98.76%.
Experimental example 1
With the SD rat is experimental subject, and extract 4.4g (the crude drug)/kg (Mus) that gives every day in the foregoing description is the administration group, dissolves gastric infusion with physiological water; After 7 days with matched group (capacity such as normal saline was irritated stomach 7 days) simultaneously vein get blood, be derivant with adenosine diphosphate sodium salt (ADP), respectively organize the platelet aggregation percentage rate by the survey of Born turbidimetry; And get cardiac blood simultaneously, and on the thrombosis appearance, forming thrombosis, the result shows; Administration group and matched group are relatively; The 1min platelet aggregation rate has obviously and reduces, and difference has statistical significance (P＜0.05), and thrombosis length also has obvious shortening (P＜0.05).Explain that extract can effectively suppress inductive platelet aggregation of ADP and the outer thrombosis of antibody, has blood circulation promoting and blood stasis dispelling, the effect of microcirculation improvement.
Experimental example 2
With the rat is experimental subject; Extract 4.4g (the crude drug)/kg (Mus) that gives every day in the foregoing description is the administration group; Dissolve gastric infusion with physiological water; Inject epinephrine simultaneously with matched group (capacity such as normal saline was irritated stomach 8 days) after 8 days and calcium chloride brings out arrhythmia, administration group has as a result been compared tangible antagonism arrhythmia effect (P＜0.05) with matched group.In experiment, find the influence of cardiac function; The extract intravenous injection is the effect of antagonism norepinephrine rising blood pressure significantly, and histamine is caused that the blood pressure reduction has certain rise effect, and wherein LVEDP, the BP index to load before and after the reflection heart all obviously reduces; And HR does not have significant change; This effect is through expansion resistance vessel and capacitance vessel, and arteriotony and left ventricular end diastolic presssure are descended, and reduces the front and back load of heart.
Experimental example 3
With the dog is experimental subject; Extract 4.4g (the crude drug)/kg (dog) that gives in the foregoing description uses physiological water dissolving gastric infusion to be the administration group; In capacity normal saline filling stomach is matched group; Irritate behind the stomach administration group and separate LCA simultaneously with matched group and survey CF and calculate coronary resistance, with Unistat type oximeter thought-read flesh oxygen consumption with MFV-110 type electromagnetic flowmeter probe.The result shows; Administration group 5min myocardial oxygen consumption, oxygen consumption index obviously reduces, and the 45min myocardial oxygen consumption descends the most remarkable after the administration; (P＜0.01 and (P＜0.001) explain that extract does not have obvious influence to the dog CF than significant difference is all arranged with reaching matched group before the administration.Heavy dose of group has the effect that reduces coronary resistance; With before the administration and matched group significant difference (P＜0.05) is more all arranged, explain that extract can reduce myocardium keto consumption, keep myocardium demand to energy; Owing to do not reduce CF, therefore improved the pump effect rate of heart.Simultaneously this medicine decreased heart rate, bring high blood pressure down, reduce effects such as coronary resistance, also help anginal alleviation.
Claims (3)
1. the extract of a Taxus mairei blade; It is characterized in that this extract is a pale yellow powder; Contain weight content in this powder and be 65～70% Ramulus et folium taxi cuspidatae flavone; Said Ramulus et folium taxi cuspidatae flavone comprises following 5 kinds of compositions: 3-O-rutin-Quercetin, 3-O-rutin-kaempferol, 3-O-rutin-myricetin, 7-O-glucose-kaempferol and 7-O-glucose-Quercetin; The gross weight content of above-mentioned 5 kinds of compositions is 40～60% in the said Ramulus et folium taxi cuspidatae flavone; This extract is a raw material with fresh southern Semen Phaseoli blade, is 40～60% alcohol solvent, stirs down that supersound extraction, extracting solution concentrating under reduced pressure go alcohol, chloroform extraction defat, water concentrate drying step to make through oven dry, crushing screening, immersion concentration.
2. the extract of the described a kind of Taxus mairei blade of claim 1 is characterized in that this extract is effective composition of medicine for cardiovascular system or health food.
3. the preparation method of extract of the described a kind of Taxus mairei blade of claim 1 is characterized in that comprising the steps:
1), be to dry 20～30 hours under 55～65 ℃ of conditions in temperature with fresh Taxus mairei blade;
2) with the Taxus mairei blade of above-mentioned oven dry be ground into can through 0.45 μ m sieve for extracting material, weigh;
3) the said extracted material is packed in the ultrasonic extraction still, add concentration again and be 40～60% ethanol, extracting material and alcoholic acid w/v (Kg/L) is 1: 15～17;
4) be under 35～55 ℃ of conditions then in temperature; Use ultrasonic sounding of independent-excited and radial vibration column transducer supersound extraction 20～30 minutes while stirring; The supersound extraction mode be each ultrasonic 3 minutes with at interval 2 minutes once ultrasonic; Ultrasonic power is 100W, and supersonic frequency is 30-70kHz, and supersound extraction is accomplished after-filtration and obtained extracting solution;
5) go pure phase at said extracted liquid elder generation concentrating under reduced pressure, the solution after will going alcohol mutually again is with the chloroform extraction defat of 3 times of volumes, and the defat water concentrate drying that finishes obtains containing the extract of the Taxus mairei blade of Ramulus et folium taxi cuspidatae flavone.
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| CN102070589B (en) * | 2010-12-24 | 2012-05-30 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting sciadopitysin from laxus malrel leaves |
| CN102093324A (en) * | 2010-12-24 | 2011-06-15 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting kayaflavone from leaves of taxus chinensis var.mairei |
| CN103044506B (en) * | 2012-12-31 | 2015-10-21 | 浙江大学宁波理工学院 | A kind of method extracting kaempferol-7-O-glucose from leaves of Taxus mairei |
| CN103030673B (en) * | 2012-12-31 | 2015-07-22 | 浙江大学宁波理工学院 | Method for extracting myricetin-3-O-rutinose from taxus mairei leaves |
| CN103059081B (en) * | 2012-12-31 | 2015-06-24 | 宁波泰新生物科技有限公司 | Method for extracting quercetin-3-O-rutinose from taxus mairei leaves |
| CN103059082B (en) * | 2012-12-31 | 2015-04-29 | 宁波泰康红豆杉生物工程有限公司 | Method for extracting taxus chinensis from taxus mairei leaves |
| CN103054912B (en) * | 2013-01-28 | 2014-12-10 | 南京中医药大学 | Taxus chinensis extractive with blood sugar reduction effect, as well as preparation method and application thereof |
| CN103349850B (en) * | 2013-07-22 | 2015-09-30 | 防城港市天红农业科技有限责任公司 | A kind of method for extracting active ingredient in wax-apple |
| CN103923138B (en) * | 2014-05-08 | 2016-03-23 | 江西天施康中药股份有限公司 | A kind of preparation method of Nicotifiorin and application thereof |
| CN104248649B (en) * | 2014-09-24 | 2017-08-18 | 江苏红豆杉药业有限公司 | A kind of preparation method and applications of Chinese yew extract |
| CN112250651B (en) * | 2020-11-12 | 2023-08-22 | 南京林业大学 | A kind of phenylpropanoid compound of yew branches and leaves and its extraction and separation method and application |
| CN116693585B (en) * | 2023-06-08 | 2024-06-21 | 大洲新燕(厦门)生物科技有限公司 | Method for preparing quercetin-7-O-beta-D-glucoside from dried orange peel and application thereof |
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