CN104189103A - Detoxicated Polygonum multiflorum Thunb extract and preparation method thereof - Google Patents
Detoxicated Polygonum multiflorum Thunb extract and preparation method thereof Download PDFInfo
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- CN104189103A CN104189103A CN201410115293.8A CN201410115293A CN104189103A CN 104189103 A CN104189103 A CN 104189103A CN 201410115293 A CN201410115293 A CN 201410115293A CN 104189103 A CN104189103 A CN 104189103A
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Abstract
A detoxicated Polygonum multiflorum Thunb extract and a preparation method thereof belong to the technical field of traditional Chinese medicines. Polygonum multiflorum Thunb coarse powder and a solvent are subjected to reflux extraction twice at the weight ratio of 1:(4-20) for 1-4 hours each time, and the solvent is reclaimed from filtrates so as to obtain a fluid extract, wherein the solvent is methyl alcohol or ethyl alcohol, and the concentration of the solvent is 30%-80%; and the Polygonum multiflorum Thunb fluid extract is diluted with water at the weight ratio of 1:(4-10), the dilution is enriched by a macroporous resin column, a solution passing through the column, a water eluate and an ethyl alcohol eluate are collected and combined, the solvent is reclaimed by pressure reduction to obtain a concentrated solution, and the concentrated solution is dried so as to obtain the detoxicated Polygonum multiflorum Thunb extract. The method provided by the invention adopts the macroporous resin separation technology to effectively remove anthraquinone components in Polygonum multiflorum Thunb to prepare the detoxicated Polygonum multiflorum Thunb extract, is simple and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of detoxification Radix Polygoni Multiflori extract, be specifically related to detoxification Radix Polygoni Multiflori extract and preparation method thereof, belong to technical field of Chinese medicines.
Technical background
Radix Polygoni Multiflori is the polygonaceae plant Radix Polygoni Multiflori (Polygonum multiflorum Thunb.) dried root, and bitter in the mouth, puckery is warm in nature.Returning liver, the heart, kidney channel, have effect of invigorating the liver and kidney, benefiting essence-blood, black beard and hair, bone and muscle strengthening, is the conventional tonic of Chinese medicine.Modern pharmacological research finds that Radix Polygoni Multiflori has slow down aging, and Fructus Alpiniae Oxyphyllae improves DNA repair function, and life-saving reduces cholesterol and improves the pharmacological actions such as lipid metabolism.Be used for the treatment of clinically the diseases such as hyperlipidemia, alopecia and weakness due to chronic disease.But in recent years, in succession occurred both at home and abroad the toxicity of a lot of Radix Polygoni Multiflori and the report of untoward reaction [1, Chen Shengjun. Radix Polygoni Multiflori hepatic injury untoward reaction information analysis and toxic mechanism progress [J] thereof. Journal of Chinese Hospital Pharmacy, 2013,07:573-577. and 2, experienced auspicious, Ke Tingting, Hu Airong. Radix Polygoni Multiflori and preparation thereof cause the routine clinical analysis of drug induced hepatic injury 52. Chinese Chinese medicine academic periodical .2013,31 (5): 1133-1134.], caused the attention of people to Radix Polygoni Multiflori toxicity.Research finds that Radix Polygoni Multiflori toxicity comes from wherein Anthraquinones chemical composition, and long-time or heavy dose is taken anthraquinone component and can be caused drug induced hepatic injury (drug-induced liver injury, DILI).For ensureing drug safety, meet the demand of people to health care, the present invention utilizes modern extraction and separation technology, prepares detoxification Radix Polygoni Multiflori extract, and this invention achievement has broad prospects and realistic meaning for the Application and Development of Radix Polygoni Multiflori.
Summary of the invention
The object of the invention is to prepare detoxification Radix Polygoni Multiflori extract.
A preparation method for detoxification Radix Polygoni Multiflori extract, is characterized in that, its preparation method is as follows:
(1) Radix Polygoni Multiflori pulverizing medicinal materials is become to coarse powder, according to Radix Polygoni Multiflori coarse powder: solvent=1:4～20(weight) ratio, reflux, extract, 2～3 times, each 1～4 hour, filtrate was reclaimed solvent, obtains fluid extract, wherein said solvent is methanol or ethanol, and concentration is 30～80%;
(2) by above-mentioned Radix Polygoni Multiflori fluid extract thin up, Radix Polygoni Multiflori fluid extract: water=1:4～10(weight), diluent is through macroporous adsorptive resins enrichment, collected post liquid, water lotion and ethanol elution, merge above solution, decompression and solvent recovery, obtains concentrated solution, concentrated solution is dry, obtains detoxification Radix Polygoni Multiflori extract.
Radix Polygoni Multiflori medical material in above-mentioned steps (1) is the polygonaceae plant Radix Polygoni Multiflori (Polygonum multiflorum Thunb.) dried root.
The every 1mL fluid extract of preferred steps (1) is with respect to crude drug 1g.
Described in above-mentioned steps (2), macroporous adsorbent resin is nonpolar or low pole macroporous adsorbent resin, is preferably D101 or AB-8 type macroporous adsorbent resin.
Described in above-mentioned steps (2), purification with macroreticular resin condition is: medical material amount is 1:1～5 with resin than (g:g), resin chromatographic column blade diameter length ratio 1:3～9, loading flow velocity 0.1～1mL/min/g resin, then use respectively deionized water and 20～60wt% ethanol water eluting, wherein the consumption of deionized water is the resin of 2～5 times of volumes, the consumption of ethanol water is 5～10 times of resin volumes, and elution flow rate is 1～3mL/min/g resin.
Purification with macroreticular resin optimum condition described in above-mentioned steps (2) is that medical material amount is 1:2 with resin than (g:g), resin chromatographic column blade diameter length ratio 1:9, loading flow velocity 0.1mL/min/g resin, then with 3 times of amounts of deionized water and 8 times of amount eluting of 40wt% ethanol, elution flow rate is 2mL/min/g resin.
In above-mentioned steps (2), drying means is that drying under reduced pressure, spraying are dried or lyophilization.
Adopt high performance liquid chromatogram to detect, testing conditions: chromatographic column is ODS chromatographic column; Mobile phase is methanol (B)-water (A), gradient elution (0～2min, 25%B～35%B; 2～10min, 35%B～50%B; 10～15min, 50%B～70%B; 15～20min, 70%B～90%B), detect wavelength and be 254 or 280nm.
The inventive method compared with prior art has following beneficial effect:
1) the inventive method is modern extraction and separation technology, good separating effect, and strong operability, is applicable to suitability for industrialized production.
2) Radix Polygoni Multiflori toxic component anthraquinone clearance can reach more than 80%.
Brief description of the drawings
Fig. 1 anthraquinone reference substance HPLC chromatogram;
Fig. 2 is embodiment 1 step (1) extracting solution HPLC chromatogram;
Fig. 3 is embodiment 1 detoxification Radix Polygoni Multiflori extract HPLC chromatogram.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
(1) Radix Polygoni Multiflori pulverizing medicinal materials is become to coarse powder, take Radix Polygoni Multiflori coarse powder 1000g, add 15 times of amount reflux, extract, of 50% ethanol 2 times, each 1.5 hours, merging filtrate, decompression recycling ethanol, to 1000mL, adds deionized water 5000mL, mixes, for subsequent use.
(2) get AB-8 type macroporous adsorbent resin 2000g, after being disposed according to macroporous adsorbent resin preprocess method, pack chromatographic column into, chromatographic column blade diameter length ratio 1:9, (1) herb liquid is added to chromatographic column, loading flow velocity is 1.0mL/min/g resin, collected post liquid simultaneously, after medicinal liquid drains off, add the deionization washing eluting of 3 times of amount resin volumes, elution flow rate is 2mL/min/g resin, collects water elution liquid, and then measures eluting with 8 times of 30% ethanol, 2mL/min/g resin, collects 30% ethanol elution.
(3) will cross post liquid, water lotion and 30% ethanol elution and merge, decompression and solvent recovery, obtains concentrated solution, and concentrated solution, through drying under reduced pressure, obtains detoxification Radix Polygoni Multiflori extract 183g.
The extract that embodiment 1 is obtained carries out high performance liquid chromatogram detection, calculates with anthraquinone chromatographic peak total peak area before and after purification, and in detoxification Radix Polygoni Multiflori extract, Anthraquinones chemical composition content is 15.77% before purification, and clearance reaches 84.23%.
Embodiment 2
(1) Radix Polygoni Multiflori pulverizing medicinal materials is become to coarse powder, take Radix Polygoni Multiflori coarse powder 100g, add 15 times of amount reflux, extract, of 40% ethanol 2 times, each 1 hour, merging filtrate, decompression recycling ethanol, to 100mL, adds deionized water 400mL, mixes, for subsequent use.
(2) get D101 type macroporous adsorbent resin 100g, after being disposed according to macroporous adsorbent resin preprocess method, pack chromatographic column into, chromatographic column blade diameter length ratio 1:6, (1) herb liquid is added to chromatographic column, loading flow velocity is 0.5mL/min/g resin, collected post liquid simultaneously, after medicinal liquid drains off, add the deionization washing eluting of 2 times of amount resin volumes, elution flow rate is 2.5mL/min/g resin, collects water elution liquid, and then measures eluting with 8 times of 50% ethanol, 2.5mL/min/g resin, collects 50% ethanol elution.
(3) will cross post liquid, water lotion and 50% ethanol elution and merge, decompression and solvent recovery, obtains concentrated solution, and concentrated solution, through drying under reduced pressure, obtains detoxification Radix Polygoni Multiflori extract 20.08g.Extract carries out high performance liquid chromatogram detection, calculates with anthraquinone chromatographic peak total peak area before and after purification, and anthraquinone clearance is not less than 82%.
Test below further illustrates the present invention:
Detection method: high performance liquid chromatography
Testing conditions: chromatographic column is Hypersil ODS(4.6 × 250mm, and 5 μ m); Mobile phase is methanol (B)-water (A), gradient elution (0～2min, 25%B～35%B; 2～10min, 35%B～50%B; 10～15min, 50%B～70%B; 15～20min, 70%B～90%B), detection wavelength is 280nm.
Anthraquinone reference substance: emodin, chrysophanic acid, chrysophanol, aloe-emodin.
Claims (10)
1. a preparation method for detoxification Radix Polygoni Multiflori extract, is characterized in that, comprises the following steps:
The ratio of (Radix Polygoni Multiflori pulverizing medicinal materials is become coarse powder by (1), according to Radix Polygoni Multiflori coarse powder: solvent=1:4～20(weight), reflux, extract, 2～3 times, each 1～4 hour, filtrate was reclaimed solvent, obtains fluid extract, wherein said solvent is methanol or ethanol, and concentration is 30～80%;
(2) by above-mentioned Radix Polygoni Multiflori fluid extract thin up, Radix Polygoni Multiflori fluid extract: water=1:4～10(weight), diluent is through macroporous adsorptive resins enrichment, collected post liquid, water lotion and ethanol elution, merge above solution, decompression and solvent recovery, obtains concentrated solution, concentrated solution is dry, obtains detoxification Radix Polygoni Multiflori extract.
2. according to the method for claim 1, it is characterized in that, Radix Polygoni Multiflori medical material described in step (1) is the polygonaceae plant Radix Polygoni Multiflori (Polygonum multiflorum Thunb.) dried root.
3. according to the method for claim 1, it is characterized in that, described in step (2), macroporous adsorbent resin is nonpolar or low pole macroporous adsorbent resin.
4. according to the method for claim 1, it is characterized in that, described macroporous adsorbent resin is D101 or AB-8 type macroporous adsorbent resin.
5. according to the method for claim 1, it is characterized in that, the every 1mL fluid extract of step (1) is with respect to crude drug 1g.
6. according to the method for claim 1, it is characterized in that, in step (2), purification with macroreticular resin condition is: medical material amount is 1:1～5 with resin than (g:g), resin chromatographic column blade diameter length ratio 1:3～9, loading flow velocity 0.1～1mL/min/g resin, then uses respectively deionized water and 20～60wt% ethanol water eluting, and wherein the consumption of deionized water is the resin of 2～5 times of volumes, the consumption of ethanol water is 5～10 times of resin volumes, and elution flow rate is 1～3mL/min/g resin.
7. according to the method for claim 6, it is characterized in that, in step (2), purification with macroreticular resin optimum condition is: medical material amount is 1:2 with resin than (g:g), resin chromatographic column blade diameter length ratio 1:9, loading flow velocity 0.1mL/min/g resin, then with 3 times of amounts of deionized water and 8 times of amount eluting of 40wt% ethanol, elution flow rate is 2mL/min/g resin.
8. according to the method for claim 1, it is characterized in that, in step (2), drying means is that drying under reduced pressure, spraying are dried or lyophilization.
9. the detoxification Radix Polygoni Multiflori extract obtaining according to the either method described in claim 1-8.
10. the detection method of the detoxification Radix Polygoni Multiflori extract obtaining according to the either method described in claim 1-8, is characterized in that, adopts high-efficient liquid phase technique, testing conditions: chromatographic column is ODS chromatographic column; Mobile phase is methanol (B)-water (A), gradient elution (0～2min, 25%B～35%B; 2～10min, 35%B～50%B; 10～15min, 50%B～70%B; 15～20min, 70%B～90%B), detect wavelength and be 254 or 280nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106474205A (en) * | 2016-12-07 | 2017-03-08 | 平凉锐博知识产权服务有限公司 | A kind of processing method of selenium-rich fleece-flower root medicine materical crude slice |
| CN113797137A (en) * | 2021-10-29 | 2021-12-17 | 浙江宜格企业管理集团有限公司 | Polygonum multiflorum extract with functions of nourishing and strengthening eyebrows and preparation method thereof |
| CN114736109A (en) * | 2022-03-02 | 2022-07-12 | 华南理工大学 | Method for selectively extracting stilbene glycoside component from Polygoni Multiflori radix |
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| CN101125154A (en) * | 2007-08-14 | 2008-02-20 | 山东轻工业学院 | Raidx cynanchum bungei decne glycoside of mountain Tai and preparation method thereof |
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- 2014-03-25 CN CN201410115293.8A patent/CN104189103A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125154A (en) * | 2007-08-14 | 2008-02-20 | 山东轻工业学院 | Raidx cynanchum bungei decne glycoside of mountain Tai and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| TING DENG,ET AL: "A dual-task method for the simultaneous detoxification and enrichment of stilbene glycoside from Polygonum multiflorum roots extract by macroporous resin", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 相聪坤: "大孔吸附树脂纯化何首乌中二苯乙烯苷的工艺研究", 《河北中医》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106474205A (en) * | 2016-12-07 | 2017-03-08 | 平凉锐博知识产权服务有限公司 | A kind of processing method of selenium-rich fleece-flower root medicine materical crude slice |
| CN113797137A (en) * | 2021-10-29 | 2021-12-17 | 浙江宜格企业管理集团有限公司 | Polygonum multiflorum extract with functions of nourishing and strengthening eyebrows and preparation method thereof |
| CN113797137B (en) * | 2021-10-29 | 2024-04-16 | 浙江宜格企业管理集团有限公司 | Polygonum multiflorum extract with functions of nourishing and strengthening eyebrows and preparation method thereof |
| CN114736109A (en) * | 2022-03-02 | 2022-07-12 | 华南理工大学 | Method for selectively extracting stilbene glycoside component from Polygoni Multiflori radix |
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