CN1660864A - Technique for preparing general flavone of Chinese globeflower with short petal some medicinal substances in high purity - Google Patents
Technique for preparing general flavone of Chinese globeflower with short petal some medicinal substances in high purity Download PDFInfo
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Abstract
A process for preparing globeflower flavone, luxtexin, vitexin and quercetin-neohesperidoside from Chinese globeflower flower includes such steps as reflux extract in alcohol solution, adsorbing by macroreticular resin, cluting, concentrating, drying to obtain globeflower flavone, and separating and purifying, luxtexin, vitexin and quercetin-neohesperioside by HSCCC.
Description
Technical field
The separation purification method of pharmaceutically active ingredient in the present invention relates to promptly provides a kind of and extracts total flavones and the preparation technology of separating and purifying high-purity Orientin, Vitexina and quercetin-3-O-neohesperidoside from total flavones from short lobe Flower of Chinese Globeflower.
Background technology
Flower of Chinese Globeflower has another name called nasturtium, is the dried floral of ranunculaceae plant Flower of Chinese Globeflower (Trollius ledebouri Reichb), is main product with northeast, North China and the Inner Mongol.Flower of Chinese Globeflower beginning sees supplementary Amplifications of the Compendium of Materia Medica, and gram-positive cocci and gram negative bacillus, alpha streptococcus, Ka Tashi mattress, Pseudomonas aeruginosa, intestinal bacteria, dysentery bacterium etc. are had the obvious suppression effect.Clinical being mainly used in treated acute appendicitis, bacillary dysentery, upper respiratory tract infection, urinary system infection etc.Its main chemical ingredients is alkaloid, flavones, organic acid, volatilization wet goods, wherein flavonoid compound is its main active ingredient, as Orientin (orientin), Vitexina (vitexin) and quercetin-3-O-neohesperidoside [hot Chunlans such as (quercetin-3-O-neohesperidoside), Pan Haifeng. the progress of Flower of Chinese Globeflower. Chengde hospital journal, 2003,20 (4): 348; Huang Wenzhe, Wang Lei, etc. short lobe Flower of Chinese Globeflower The Chemical Constituents. herbal medicine, 2000,31 (10): 731; Kang Shaowen, Yu Yongfang, etc. the Flower of Chinese Globeflower The Chemical Constituents. herbal medicine, 1984,15 (6): 247].Their structural formula is as follows:
Orientin
Vitexina
Quercetin-3-O-neohesperidoside
With the purification with macroreticular resin total flavones of tropaeolum report is also arranged, but gained general flavone content lower (being lower than 40%) is not seen the report that has the preparative chromatography technology to be used for the preparation of Flower of Chinese Globeflower high-purity monomer compound separation simultaneously, also not seeing has relevant patent.
At present, mostly be the effective monomer that adopts in traditional method for separating and preparing separating plant such as column chromatography and recrystallization both at home and abroad, waste time and energy, contaminate environment [C.L Ky, M.Noirot, S.Hamon, J.Agric.Food.Chem.1997,45:786; W.M.Yan, Acta Botanica Sinica, 1979,20:54; J.J Liu, G.L.Zhao, H.Wang, X.H.Zhang, J.Cent.South.Univ.T.2002,9:246], and used stationary phase has weak points such as non-reversibility adsorption to sample.
Therefore, people solve the problems referred to above to the isolation technique that adopts better effects and if have demand.The purpose of this invention is to provide a kind of from short lobe Flower of Chinese Globeflower dna purity be higher than 60% the total flavones and the preparation technology of several high purity medical monomer (Orientin, Vitexina and quercetin-3-O-neohesperidoside).
High speed adverse current chromatogram (High-speed counter-current chromatography HSCCC) is a kind of newer liquid liquid distribution chromatography technology, it need not any solid support or carrier and overcome the non-reversibility adsorption of traditional separation method to sample, thereby sample recovery rate height, also have advantages such as applied range, instrumentation is simple, fractional dose is big simultaneously, therefore be widely used in the middle of the separation preparation of natural product.We adopt high-speed countercurrent chromatography to prepare purity to be higher than 98% Orientin, Vitexina and purity be 85% quercetin-3-O-neohesperidoside, and be further purified by preparative liquid chromatography and obtained purity and be higher than 98% quercetin-3-O-neohesperidoside.
Summary of the invention
In order to solve the problems of the technologies described above, technical scheme of the present invention is as follows:
A kind ofly from short lobe Flower of Chinese Globeflower, extract total flavones and separating and purifying high-purity Orientin from total flavones, the method of Vitexina and quercetin-3-O-neohesperidoside, specifically comprise: medicinal material extract, the separation and purification three process of total flavones preparation and monomeric compound, it is characterized in that in the medicinal material extract operation (1), to lack the lobe Flower of Chinese Globeflower with 50%～70% medicinal alcohol refluxing extraction, obtain extracting solution behind the decompression recycling ethanol, in the total flavones preparation section (2), extracting solution is crossed macroporous adsorbent resin, water and 25%～35% medicinal alcohol wash-out, can get total flavones behind the ethanol eluate concentrate drying, in the monomeric compound separation and purification operation (3), adopt high-speed countercurrent chromatography that the gained total flavones is carried out separation and purification, it comprises that preparation constitutes the high speed adverse current chromatogram stationary phase, the solvent system of moving phase, make in the counter current chromatograph pillar and be full of stationary phase, pillar is rotated, again moving phase is pumped in the post, enter the crude extract sample for preparing by sampling valve, according to detector spectrogram receiving target composition " I ", " II ", " III ", and use preparative liquid chromatography once more separation and purification stream part " I " obtain stream part " IV ".
Operation (1) medicinal material extract
Get dry globeflower medicinal materials with 50%～70% alcohol reflux 2 times, each 2 hours, filter, merging filtrate, concentrating under reduced pressure (60 ℃) they are the extracting solution after concentrating to there not being the alcohol flavor.
The preparation of operation (2) total flavones
After getting extracting solution after concentrating and adding the suitable quantity of water suspendible, cross macroporous adsorbent resin, water and 25%～35% ethanol elution can get purity after the ethanol elution stream part concentrating under reduced pressure drying (60 ℃) and be higher than 60% total flavones of tropaeolum.
Operation (3) monomeric compound separation and purification
Use high speed adverse current chromatogram total flavones is carried out separation and purification, it comprises that preparation constitutes the solvent system of stationary phase, moving phase, make in the counter current chromatograph pillar and be full of stationary phase, pillar is rotated, moving phase is pumped in the post, the solvent for use system is made up of ethyl acetate, propyl carbinol, water again, and amount ratio is 2: 1: 3, by the sampling valve sample introduction, according to detecting spectrogram receiving target composition " I ", " II ", " III ".This method can prepare stream part " I " of containing 85% quercetin-3-O-neohesperidoside and be higher than stream part " II " (Orientin), stream part " III " (Vitexina) of 98% with purity.
Preparation liquid phase separation purifying
Use preparative liquid chromatography to being further purified, can get purity and be higher than 98% quercetin-3-O-neohesperidoside, be i.e. stream part " IV " through high speed adverse current chromatogram separation and purification gained stream part " I ".
The purity detecting of isolate and structure are identified, adopt high performance liquid chromatography to carry out purity detecting (peak area normalization method) to getting component, volatilize carry out behind the solvent MS,
1HNMR and
13CNMR analyzes, and carries out structural confirmation according to the gained data.
The present invention adopts high speed adverse current chromatogram and preparative liquid chromatography in conjunction with the Chinese medicine crude extract is carried out separation and purification, and is easy, quick, also avoided sample loss simultaneously.Overcome shortcomings such as traditional preparation process method complex operation, separation cycle be long, and have that preparation amount is big, separation efficiency is high, good product purity, advantage such as simple and easy to do, be easy to promote the use of.
Description of drawings
Fig. 1 is total flavones of tropaeolum preparation flow figure
Fig. 2 is the color atlas of total flavones of tropaeolum half countercurrent chromatography (HSCCC)
Fig. 3 is the color atlas of quercetin-3-O-neohesperidoside preparative liquid chromatography
Fig. 4-1 is the color atlas of total flavones of tropaeolum high performance liquid chromatography (HPLC)
Fig. 4-2 is the color atlas of the separating obtained stream of high-speed counter-current part " II " (Orientin) high performance liquid chromatography (HPLC)
Fig. 4-3 is the color atlas of the separating obtained stream of high-speed counter-current part " III " (Vitexina) high performance liquid chromatography (HPLC)
Fig. 4-4 is the color atlas of high-speed counter-current part from gained stream part " I " (the stream part that contains quercetin-3-O-neohesperidoside) high performance liquid chromatography (HPLC)
Fig. 4-5 is the color atlas of preparative liquid chromatography stream part " IV " (quercetin-3-O-neohesperidoside) high performance liquid chromatography (HPLC).
Embodiment
The present invention will be described below in conjunction with specific embodiment and accompanying drawing
Embodiment 1:
Shown in Fig. 1 total flavones of tropaeolum preparation flow figure
1. medicinal material extract: take by weighing dry globeflower medicinal materials 300g, with 10 times of amount 60% alcohol reflux 2 times, each 2 hours, filter, merging filtrate, concentrating under reduced pressure (60 ℃) is to not having alcohol flavor, the extracting solution after must concentrating.
2. total flavones preparation: get the extracting solution after concentrating, add (cumulative volume is 900ml) behind the water suspendible.Join and 500g is housed on the chromatography column of 1300 pretreated macroporous adsorbent resins, absorption was 1.0 hours after last sample finished.With 1200ml water elution (discarding).Use 2000ml 30% medicinal alcohol wash-out again, behind the ethanol elution stream part concentrating under reduced pressure, vacuum-drying (60 ℃) gets total flavones powder 16.7g, and extracting yield is 5.57%, and total flavones purity is 61.6%.
3. the separation and purification of monomeric compound:
3.1 use high speed adverse current chromatogram (Shenzhen is with the biochemical company limited in field product) separation and purification total flavones.Solvent system and consumption volume ratio are ethyl acetate: propyl carbinol: water=2: 1: 3, on be stationary phase mutually, be moving phase mutually down, the adverse current chromatogram column volume is 300ml, stationary phase retention rate 47%, flow velocity 2.0ml/min, rotating speed 800rpm, detect wavelength 254nm, get during total flavones powder 500mg is dissolved under the 15ml mutually, behind the sample introduction in the case the color atlas of record see Fig. 2.
Concrete operation steps is: than the preparation solvent system, static layering behind the shake well in separating funnel is divided and is got phase up and down by above-mentioned solvent volume, on be stationary phase mutually, under be moving phase mutually.Make earlier in the counter current chromatograph pillar to be full of stationary phase, main frame is rotated, pump into moving phase again, by the sampling valve sample introduction, according to detector spectrogram receiving target composition " I ", " II ", " III ".
The purity detecting of isolate and structure are identified, adopt high performance liquid chromatography to carry out purity detecting (peak area normalization method) to getting component, volatilize carry out behind the solvent MS,
1HNMR and
13CNMR analyzes, and carries out structural confirmation according to the gained data.
Show that through high-efficient liquid phase analysis stream part " II ", " III " are single chromatographic peak, peak purity is respectively 99.6%, 98.1%, and peak purity is 85.1% in the stream part " I ".Show that through the structure evaluation stream part " II " is Orientin, " III " is Vitexina.
3.2 use preparative liquid chromatography separation and purification stream part " I ".Chromatographic condition is: 0.1% aqueous acetic acid: tetrahydrofuran (THF): Virahol: acetonitrile (460: 30: 20: 10); Flow velocity: 3.0ml/min; Chromatographic column: YWG C
18(10.0 * 200mm i.d.10 μ m), column temperature: 30 ℃, detect wavelength: 254nm.According to detector spectrogram receiving target composition, promptly stream part " IV " carries out high-efficient liquid phase analysis to this stream part and shows that it is single chromatographic peak, and peak purity is 98.3%.Preparative liquid chromatography figure sees Fig. 3.Show that through the structure evaluation stream part " IV " is quercetin-3-O-neohesperidoside.
HPLC analysis condition: chromatographic column: Hypersil C
18(4.0 * 200mm i.d.5 μ m); Moving phase: 0.05% phosphate aqueous solution: tetrahydrofuran (THF): Virahol: acetonitrile (420: 30: 20: 30); Flow velocity: 0.5ml/min; Column temperature: 30 ℃, detect wavelength: 254nm.Total flavones, high speed adverse current chromatogram and preparative liquid chromatography separate part color atlas see that Fig. 4-1 is to Fig. 4-5 (peak 1 is quercetin-3-O-neohesperidoside, and peak 2 is an Orientin, and peak 3 is a Vitexina) with this understanding.Wherein Fig. 4-1 is the total flavones color atlas, Fig. 4-2 is HSCCC separated flow part " II " (Orientin) color atlas, Fig. 4-3 is HSCCC separated flow part " III " (Vitexina) color atlas, Fig. 4-4 is stream part color atlas " I " (high-speed counter-current part contains stream part of quercetin-3-O-neohesperidoside from gained), and Fig. 4-5 is preparative liquid chromatography stream part " IV " (quercetin-3-O-neohesperidoside) color atlas.
Structure is identified: quercetin-3-O-neohesperidoside, Orientin and Vitexina that separation is obtained carry out on VarianINOVA-500 type nuclear magnetic resonance analyser and Varian MAT-212 type mass spectrograph
1HNMR,
13CNMR and MS analyze, and the gained data are as follows.
Orientin, yellow powder, UV λ max (nm MeOH): 345,270,255.ESI-MS:448 (M
+), 430 (M-H
2O), 412 (M-2H
2O), 394 (M-3H
2O), 299 (aglycon+CH
2 +).
1HNMR(500MHz，DMSO-d
6)δ：4.92(1H，d，J＝10.0Hz，H-1″)，6.51(1H，s，H-6)，6.88(1H，s，H-3)，7.10(1H，d，J＝8.0Hz，H-5＇)，7.50～7.94(2H，m，H-2′，6′)，13.55(1H，brs，5-OH)。
13CNMR(500MHz，DMSO-d
6)δ：163.01(C-2)，103.99(C-3)，182.03(C-4)，160.47(C-5)，98.31(C-6)，164.16(C-7)，104.65(C-8)，156.27(C-9)，102.41(C-10)，121.97(C-1′)，114.07(C-2′)，145.95(C-3′)，149.90(C-4′)，115.78(C-5′)，119.45(C-6′)，73.50(C-1″)，70.90(C-2″)，78.88(C-3″)，70.83(C-4″)，82.04(C-5″)，61.76(C-6″)。
Vitexina, yellow powder, UV λ max (nm MeOH): 330,301 (shoulders), 269.ESI-MS:432 (M
+), 414 (M-H
2O), 396 (M-2H
2O), 283 (aglycon+CH
2 +).
1HNMR (500MHz, DMSO-d
6) δ: 3～4 (6H, m, protons on the sugar), 4.94 (1H, d, J=10.0Hz, H-1 "), 6.54 (1H, s, H-6), 7.04 (1H; s, H-3), 7.15 (2H, d, J=8.0Hz; H-3 ', 5 '), 8.26 (2H, d, H-2 '; 6 '), 10.35 (1H, s, 4 '-OH), 10.83 (1H; s, 7-OH), 13.17 (1H, s, 5-OH).
13CNMR(500MHz，DMSO-d
6)δ：162.98(C-2)，104.51(C-3)，182.73(C-4)，156.64(C-5)，98.95(C-6)，164.31(C-7)，104.56(C-8)，160.28(C-9)，105.07(C-10)，122.07(C-1′)，128.99(C-2′，6′)，115.01(C-3′，5′)，161.32(C-4′)，73.93(C-1″)，71.03(C-2″)，79.01(C-3″)，70.20(C-4″)，81.99(C-5″)，61.76(C-6″)。
Quercetin-3-O-neohesperidoside, yellow powder, ESI-MS:610 (M
+), 301 (aglycons).
1HNMR (500MHz, DMSO-d
6) δ: 1.44 (3H, d, rha-CH
3), 3.90～4.47 (10H, m, protons on the sugar), 5.27 (1H, d, rha-C
1-H), 5.93 (1H, d, GluC
1-H), 6.55 (1H, d, J=2Hz, H-6), 6.59 (1H, d, J=2.0Hz, H-8), 7.28 (1H, d, J=8.0Hz, H-5 '), 8.04 (1H, dd, J=2.0Hz, J=8.0Hz, H-6 '), 8.26 (2H, d, H-2 ').13CNMR(500MHz，DMSO-d6)δ：146.94(C-2)，134.08(C-3)，177.88(C-4)，156.32(C-5)，98.28(C-6)，164.02(C-7)，93.44(C-8)，160.94(C-9)，103.27(C-10)，135.96(C-1′)，115.84(C-2′)，147.95(C-3′)，145.18(C-4′)，115.16(C-5′)，120.15(C-6′)，99.4(C-1″)，77.6(C-2″)，77.4(C-3″)，69.6(C-4″)，77.1(C-5″)，60.5(C-6″)，100.7(C-1)，70.6(C-2)，71.3(C-3)，70.9(C-4)，71.7(C-5)，18.1(C-6)。
Embodiment 2:
1. take by weighing dry globeflower medicinal materials 300g, with 10 times of amount 50% alcohol reflux 2 times, each 2 hours, filter, merging filtrate, concentrating under reduced pressure (60 ℃) is to not having alcohol flavor, the extracting solution after must concentrating.
2. get the extracting solution after concentrating, add that cumulative volume is 900ml behind the water suspendible.Join and 500g is housed on the chromatography column of pretreated AB-8 type macroporous adsorbent resin, absorption was 1.0 hours after last sample finished.With 1400ml water elution (discarding).Use 2200ml 25% medicinal alcohol wash-out again, behind the ethanol elution stream part concentrating under reduced pressure, vacuum-drying (60 ℃) gets amount of powder 16.3g, and yield is 5.43%, and total flavones purity is 62.2%.
3. method, step and result thereof that the separation and purification of quercetin-3-O-neohesperidoside, Orientin and Vitexina in the total flavones, purity detecting and structure are identified are with example 1.
Embodiment 3:
1. take by weighing dry globeflower medicinal materials 300g, with 10 times of amount 70% alcohol reflux 2 times, each 2 hours, filter, merging filtrate, concentrating under reduced pressure (60 ℃) is to not having alcohol flavor, the extracting solution after must concentrating.
2. get the extracting solution after concentrating, add that cumulative volume is 900ml behind the water suspendible.Join and 500g is housed on the chromatography column of pretreated AB-8 type macroporous adsorbent resin, absorption was 1.0 hours after last sample finished.With 1400ml water elution (discarding).Use 2000ml 35% medicinal alcohol wash-out again, behind the ethanol elution stream part concentrating under reduced pressure, vacuum-drying (60 ℃) gets total flavones amount of powder 18.6g, and yield is 6.20%, and total flavones purity is 63.3%.
3. method, step and result thereof that the separation and purification of quercetin-3-O-neohesperidoside, Orientin and Vitexina in the total flavones, purity detecting and structure are identified are with example 1.
Claims (5)
1. one kind is extracted total flavones and separating and purifying high-purity Orientin from total flavones from short lobe Flower of Chinese Globeflower, the method of Vitexina and quercetin-3-O-neohesperidoside, specifically comprise: medicinal material extract, the separation and purification three process of total flavones preparation and monomeric compound, it is characterized in that in the medicinal material extract operation (1), to lack the lobe Flower of Chinese Globeflower with 50%～70% medicinal alcohol refluxing extraction, obtain extracting solution behind the decompression recycling ethanol, in the total flavones preparation section (2), extracting solution is crossed macroporous adsorbent resin, water and 25%～35% medicinal alcohol wash-out, can get total flavones behind the ethanol eluate concentrate drying, in the monomeric compound separation and purification operation (3), adopt high-speed countercurrent chromatography that the gained total flavones is carried out separation and purification, it comprises that preparation constitutes the high speed adverse current chromatogram stationary phase, the solvent system of moving phase, make in the counter current chromatograph pillar and be full of stationary phase, pillar is rotated, again moving phase is pumped in the post, enter the total flavones sample for preparing by sampling valve, according to detector spectrogram receiving target stream part " I ", " II ", " III ", and use preparative liquid chromatography convection current part " I " and be further purified, obtain stream part " IV ".
2. a kind ofly from short lobe Flower of Chinese Globeflower, extract total flavones and the method for separating and purifying high-purity Orientin, Vitexina and quercetin-3-O-neohesperidoside from total flavones according to claim 1 is described, it is characterized in that in the medicinal material extract operation (1), to lack the lobe Flower of Chinese Globeflower and measure 60% medicinal alcohol refluxing extraction 2 times, obtain extracting solution behind the decompression recycling ethanol with 10 times.
3. a kind ofly from short lobe Flower of Chinese Globeflower, extract total flavones and the method for separating and purifying high-purity Orientin, Vitexina and quercetin-3-O-neohesperidoside from total flavones according to claim 1 is described, it is characterized in that in the total flavones preparation section (2) that the macroporous adsorbent resin model can be 1300 or AB-8 type macroporous adsorbent resin, water and 30% medicinal alcohol wash-out can get total flavones behind the ethanol eluate concentrate drying.
4. a kind ofly from short lobe Flower of Chinese Globeflower, extract total flavones and the method for separating and purifying high-purity Orientin, Vitexina and quercetin-3-O-neohesperidoside from total flavones according to claim 1 is described, it is characterized in that in the monomeric compound separation and purification operation (3), use high-speed countercurrent chromatography total flavones is carried out separation and purification, used two-phase solvent system is an ethyl acetate: propyl carbinol: water, two-phase solvent system ethyl acetate: propyl carbinol: the best proportioning of water is 2: 1: 3.
5. describedly a kind ofly from short lobe Flower of Chinese Globeflower, extract total flavones and the method for separating and purifying high-purity Orientin, Vitexina and quercetin-3-O-neohesperidoside from total flavones according to claim 1 or 4, it is characterized in that using preparative liquid chromatography high speed adverse current chromatogram gained stream part " I " is further purified, obtain pure product.
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| CN100473658C (en) * | 2006-08-09 | 2009-04-01 | 江苏省中国科学院植物研究所 | Method of extracting and purifying sphenomeris chinensis orientin and vitexin |
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| CN106038713A (en) * | 2016-08-02 | 2016-10-26 | 新疆维吾尔自治区药物研究所 | Nymphaea candida presl total flavonoid extract as well as preparation method and application thereof |
| CN106038713B (en) * | 2016-08-02 | 2019-11-12 | 新疆维吾尔自治区药物研究所 | Nymphaea tetragona extractive of general flavone and its preparation method and application |
| CN110025679A (en) * | 2019-04-19 | 2019-07-19 | 上海应用技术大学 | A kind of preparation method of Trollius ledebouri antioxidant extract |
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