CN104098636A - Method for extracting rutin from Japanese pagoda tree flowers - Google Patents
Method for extracting rutin from Japanese pagoda tree flowers Download PDFInfo
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- CN104098636A CN104098636A CN201410390877.6A CN201410390877A CN104098636A CN 104098636 A CN104098636 A CN 104098636A CN 201410390877 A CN201410390877 A CN 201410390877A CN 104098636 A CN104098636 A CN 104098636A
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- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 title claims abstract description 57
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 title claims abstract description 57
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 title claims abstract description 57
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 title claims abstract description 57
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 235000005493 rutin Nutrition 0.000 title claims abstract description 57
- 229960004555 rutoside Drugs 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 27
- 235000010586 Sophora japonica Nutrition 0.000 title abstract description 7
- 241000219785 Styphnolobium japonicum Species 0.000 title abstract 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 239000012043 crude product Substances 0.000 claims abstract description 15
- 229920001213 Polysorbate 20 Polymers 0.000 claims abstract description 13
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims abstract description 13
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims abstract description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 11
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000007670 refining Methods 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims description 36
- 241000219784 Sophora Species 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 9
- 229910021538 borax Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000004328 sodium tetraborate Substances 0.000 claims description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000002525 ultrasonication Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 2
- 235000019441 ethanol Nutrition 0.000 abstract 2
- 238000010025 steaming Methods 0.000 abstract 1
- 239000013543 active substance Substances 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 208000007530 Essential hypertension Diseases 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 244000046101 Sophora japonica Species 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
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- -1 flavonoid glycoside compound Chemical class 0.000 description 1
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- 210000003677 hemocyte Anatomy 0.000 description 1
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- 238000000874 microwave-assisted extraction Methods 0.000 description 1
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Abstract
The invention discloses a novel method for extracting rutin from Japanese pagoda tree flowers. The method for extracting the rutin from the Japanese pagoda tree flowers comprises the following steps of processing dried Japanese pagoda tree flowers under 70 DEG C through a drying steaming method and airing and smashing the Japanese pagoda tree flowers; adding surface active agent with the reasonable ratio such as Tween 20 and OP-15, performing ultrasonic-assisted extraction through ethyl alcohol with the alcohol concentration to be from 60 to 70 % under a certain condition, standing extraction solution to be crystallized and obtaining rutin crude products through suction filtration; refining the rutin crude products through n-butyl alcohol, standing the rutin crude products to be crystallized and drying under 130 DEG C to obtain rutin products with the purity to be more than 98 %, wherein the yield is larger than 22 %. The method for extracting the rutin from the Japanese pagoda tree flowers is simple in operation, high in extraction efficiency and applicable to product and reality.
Description
Technical field
The application relates to a kind of method of extracting rutin from the sophora bud.
Background technology
The sophora bud is the dry flower and alabastrum of leguminous plants Chinese scholartree, the history of being used as medicine existing more than 2000 year, and < < Shennong Bencaojing > > is classified as top grade.The rutin containing in the sophora bud approximately 8%～28%(according to the sophora bud place of production and collect the difference of time and difference to some extent).Rutin claims again violaguercitrin, rutin, belongs to flavonoid glycoside compound, has cooling blood for hemostasis, the effect of clearing liver-fire, can reduce capillary permeability and fragility, promote hyperplasia and prevent that hemocyte from condensing, also have anti-inflammatory, antianaphylaxis, diuresis, antibechic, reducing blood-fat etc. effect.Rutin clinically as the assisting therapy of essential hypertension, prevent because rutin lacks other hemorrhages that cause and prevention and treatment diabetes and merge hyperlipidemia.In addition, rutin is as natural antioxidant and use yellow pigment, is also widely used in protective foods and cosmetic kind.
In prior art, common rutin extraction method has that boiling water decocts, alkali carries heavy, the ultrasonic or microwave extraction of acid, Soxhlet extraction, supercritical CO
2extract etc.Common purification process has crystallization, macroporous adsorbent resin processing, high performance liquid chromatography processing etc.; Along with tensio-active agent being widely used in fields such as chemical industry, food, daily necessities production and water treatments, water insoluble or not soluble in water effective constituent in a lot of Chinese medicine, as Flavonoid substances, alkaloid, volatilization wet goods, can on its surface or interface, form adsorption by tensio-active agent, or in solution, form molecule aggregation body, and then change the solvability of these compositions in the aqueous solution, improved the extraction efficiency of Chinese medicine, reduced extraction cost, the feature of safety and environmental protection.In prior art, there is the report that adopts the auxiliary Extraction of rutin of tensio-active agent, but adopt a kind of tensio-active agent more.As (" the improvement researchs of Rutin Extracting Technology " such as Li Jinxiu, Li Jinxiu, Gong Shengzhao, Huang Qiujin, Guangdong chemical industry, the 1st phase in 2003, P15) adopted following methods to carry out the extraction of violaguercitrin: the sophora bud is pulverized, the water that adds 5 times of amounts, with liming, regulate pH8～9, in temperature, be 50～60 ℃ and extract 20～30min, filter, by similarity condition, repeatedly extract 3 times, filtrate is 3 with salt acid for adjusting pH, add 0.5% Surfactant OP, at 60～70 ℃ of insulation 10min, standing 30min, filter, washing, dry, obtain violaguercitrin product yield 18.4%, content 96%.
Summary of the invention
The application aims to provide a kind of new method of extracting rutin from the sophora bud.
The method of the invention comprises the following steps:
(1) pre-treatment: will be dried the sophora bud and process 30min with dry blowing method at 70 ℃, then go out colloid with 70 ℃ of hot water drip washing, and dried afterwards and pulverize the order into 20-80;
(2) extract: sophora bud particle is added to 1～5% borax, 1～5% Na
2sO
3in 15-30 60～70% ethanol doubly, use sodium bicarbonate to regulate pH to 9～10, add again 0.3～0.5% Tween 20 and 0.05～0.3% OP-15, lucifuge ultrasonic extraction 10～30min under 20～30kHz, the condition of 30～50 ℃, filter afterwards, filtrate lucifuge at 30～50 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 30～50 ℃, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20～30min, suction filtration obtains rutin crude product;
(3) refining: rutin crude product is placed in to baking oven, at 40 ℃, dry extremely without alcohol taste, be warming up to gradually again 130 ℃ of oven dry, the dry rutin obtaining is added in propyl carbinol and is heated to dissolve, filter, in filtrate, add deionized water, adopt 20～30kHz ultrasonic at 0～5 ℃ lucifuge process 20～30min, standing crystallization is also dried at 130 ℃, obtains more than 98% rutin of purity, and yield reaches more than 22%.
Further, in step of the present invention (2), preferably add 3～4% borax and 1% Na
2sO
3.
Further, in step of the present invention (2), preferably add 0.35～0.45% Tween 20 and 0.05～0.2% OP-15.
Further, in step of the present invention (2), the condition optimization of ultrasonic extraction extracts 15～25min at 30kHz, 40～50 ℃.
Further, in step of the present invention (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; The condition optimization of ultrasonication is processed 20～30min under 30 kHz.
Further, in step of the present invention (2), be more preferably and add 0.35～0.45% Tween 20 and 0.05～0.15% OP-15.
The present invention has used tensio-active agent Tween 20 and the OP-15 of rational proportion in extraction step, and the tensio-active agent of this proportioning makes extraction time and crystallization time all have shortening, and extraction efficiency improves, then is aided with ultrasonic wave, and yield is increased obviously.Adopt propyl carbinol to refine rutin, can effectively remove the impurity such as residual colloid, lipid acid, improve the purity of rutin.Comprehensive each step of the present invention, the method for the invention is easy and simple to handle, and extraction efficiency is high, is applicable to produce actual.
Accompanying drawing explanation
Fig. 1 is rutin standard substance HPLC spectrogram.
Fig. 2 is the HPLC spectrogram of rutin end product in embodiment 2.
Embodiment
Embodiment 1
The dry sophora bud of 50g is processed to 30min with dry blowing method at 70 ℃, then go out colloid with 70 ℃ of hot water drip washing, being dried afterwards and pulverizing is 20 orders.Sophora bud particle is added to 3% borax, 1% Na
2sO
3in 60～70% ethanol of 20 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.35% Tween 20 and 0.15% OP-15, lucifuge ultrasonic extraction 20min under 30kHz, the condition of 40 ℃, filters afterwards, and filtrate lucifuge at 40 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, the filtrate obtaining and filtrate merging before; In the filtrate after merging, add 5% gac, lucifuge stirs 10min at 40 ℃, and the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20min, and suction filtration obtains rutin crude product.Rutin crude product is placed in to baking oven, at 40 ℃, dry extremely without alcohol taste, be warming up to gradually again 130 ℃ of oven dry, the dry rutin obtaining is added in 1300mL propyl carbinol and is heated to dissolve, filter, in filtrate, add 130mL deionized water, adopt 30kHz ultrasonic at 0～5 ℃ lucifuge process 20min, standing crystallization, leaches rear 130 ℃ of oven dry, obtain the rutin 11.38g of purity 98.66%, yield 22.76%.
Embodiment 2
The dry sophora bud of 80g is processed to 30min with dry blowing method at 70 ℃, then go out colloid with 70 ℃ of hot water drip washing, being dried afterwards and pulverizing is 40 orders.Sophora bud particle is added to 4% borax, 1% Na
2sO
3in 60～70% ethanol of 25 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.40% Tween 20 and 0.10% OP-15, lucifuge ultrasonic extraction 20min under 30kHz, the condition of 40 ℃, filters afterwards, and filtrate lucifuge at 40 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, the filtrate obtaining and filtrate merging before; In the filtrate after merging, add 5% gac, lucifuge stirs 10min at 40 ℃, and the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20min, and suction filtration obtains rutin crude product.Rutin crude product is placed in to baking oven, at 40 ℃, dry extremely without alcohol taste, be warming up to gradually again 130 ℃ of oven dry, the dry rutin obtaining is added in 2L propyl carbinol and is heated to dissolve, filter, in filtrate, add 200mL deionized water, adopt 30kHz ultrasonic at 0～5 ℃ lucifuge process 20min, standing crystallization, leaches rear 130 ℃ of oven dry, obtain the rutin 18.57g of purity 98.81%, yield 23.21%.
Embodiment 3
The dry sophora bud of 120g is processed to 30min with dry blowing method at 70 ℃, then go out colloid with 70 ℃ of hot water drip washing, being dried afterwards and pulverizing is 60 orders.Sophora bud particle is added to 3% borax, 1% Na
2sO
3in 60～70% ethanol of 30 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.45% Tween 20 and 0.05% OP-15, lucifuge ultrasonic extraction 20min under 30kHz, the condition of 40 ℃, filters afterwards, and filtrate lucifuge at 40 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, the filtrate obtaining and filtrate merging before; In the filtrate after merging, add 5% gac, lucifuge stirs 10min at 40 ℃, and the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20min, and suction filtration obtains rutin crude product.Rutin crude product is placed in to baking oven, at 40 ℃, dry extremely without alcohol taste, be warming up to gradually again 130 ℃ of oven dry, the dry rutin obtaining is added in 3L propyl carbinol and is heated to dissolve, filter, in filtrate, add 300mL deionized water, adopt 30kHz ultrasonic at 0～5 ℃ lucifuge process 20min, standing crystallization, leaches rear 130 ℃ of oven dry, obtain the rutin 27.16g of purity 98.86%, yield 22.63%.
Embodiment 4
The present embodiment has contrasted and in Extraction of rutin step, has used the tensio-active agent of proportioning of the present invention and use separately the impact of Tween 20 on rutin finished product productive rate and purity.First the dry sophora bud of 50g is processed with the pretreatment process described in the embodiment of the present application 1.Extraction step is operating as: by pulverizing, be that 20 object sophora bud particles join 3% borax, 1% Na
2sO
3in 60～70% ethanol of 20 times, use sodium bicarbonate to regulate pH to 9～10, then add 0.5% Tween 20, lucifuge ultrasonic extraction 20min under 30kHz, the condition of 40 ℃, filters afterwards, and filtrate lucifuge at 40 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, the filtrate obtaining and filtrate merging before; In the filtrate after merging, add 5% gac, lucifuge stirs 10min at 40 ℃, and the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20min, and suction filtration obtains rutin crude product.With the process for purification described in the embodiment of the present application 1, rutin crude product is refined again afterwards.More than operation is done respectively 2 groups of parallel check experiments with method described in embodiment 1, and quality and the purity of the rutin end product obtaining are contrasted, and result is as shown in the table:
Claims (8)
1. from the sophora bud, extract a method for rutin, it is characterized in that comprising the following steps:
(1) pre-treatment: will be dried the sophora bud and process 30min with dry blowing method at 70 ℃, then go out colloid with 70 ℃ of hot water drip washing, and dried afterwards and pulverize the order into 20-80;
(2) extract: sophora bud particle is added to 1～5% borax, 1～5% Na
2sO
3in 15-30 60～70% ethanol doubly, use sodium bicarbonate to regulate pH to 9～10, add again 0.3～0.5% Tween 20 and 0.05～0.3% OP-15, lucifuge ultrasonic extraction 10～30min under 20～30kHz, the condition of 30～50 ℃, filter afterwards, filtrate lucifuge at 30～50 ℃ is standby; Filter residue extracts once with above-mentioned same condition again, and the filtrate obtaining merges with filtrate before, in the filtrate after merging, adds 5% gac, at 30～50 ℃, lucifuge stirs 10min, the filtrate of filtering after carbon removal is acidified to pH=3～4, standing 20～30min, suction filtration obtains rutin crude product;
(3) refining: rutin crude product is placed in to baking oven, at 40 ℃, dry extremely without alcohol taste, be warming up to gradually again 130 ℃ of oven dry, the dry rutin obtaining is added in propyl carbinol and is heated to dissolve, filter, in filtrate, add deionized water, adopt 20～30kHz ultrasonic at 0～5 ℃ lucifuge process 20～30min, standing crystallization is also dried at 130 ℃, obtains more than 98% rutin of purity, and yield reaches more than 22%.
2. the method for extraction as claimed in claim 1 rutin, is characterized in that: in described step (2), add 3～4% borax and 1% Na
2sO
3.
3. the method for extraction as claimed in claim 1 or 2 rutin, is characterized in that: in described step (2), add 0.35～0.45% Tween 20 and 0.05～0.2% OP-15.
4. the method for extraction as claimed in claim 1 or 2 rutin, is characterized in that: in described step (2), and ultrasonic extraction 15～25min under 30kHz, 40～50 ℃ of conditions.
5. the method for extraction rutin as claimed in claim 1 or 2, is characterized in that: in described step (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; Ultrasonication 20～30min under 30 kHz conditions.
6. the method for extraction as claimed in claim 3 rutin, is characterized in that: in described step (2), add 0.35～0.45% Tween 20 and 0.05～0.15% OP-15.
7. the method for extraction as claimed in claim 6 rutin, is characterized in that: in described step (2), and ultrasonic extraction 15～25min under 30kHz, 40～50 ℃ of conditions.
8. the method for extraction rutin as claimed in claim 6, is characterized in that: in described step (3), adding the volume of propyl carbinol and the ratio of sophora bud raw materials quality is 20～30mL/g; Adding the volume of deionized water and the ratio of sophora bud raw materials quality is 2～3mL/g; Ultrasonication 20～30min under 30 kHz conditions.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558073A (en) * | 2014-12-26 | 2015-04-29 | 苏州亚宝药物研发有限公司 | Preparation method of rutin |
| CN106397513A (en) * | 2016-10-27 | 2017-02-15 | 广西禅方药业股份有限公司 | Method for refining rutin having content more than or equal to 98% |
| CN115109108A (en) * | 2022-06-21 | 2022-09-27 | 云南八凯农业开发有限公司 | Method for extracting buckwheat rutin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558073A (en) * | 2014-12-26 | 2015-04-29 | 苏州亚宝药物研发有限公司 | Preparation method of rutin |
| CN104558073B (en) * | 2014-12-26 | 2017-10-03 | 苏州亚宝药物研发有限公司 | A kind of preparation method of rutin |
| CN106397513A (en) * | 2016-10-27 | 2017-02-15 | 广西禅方药业股份有限公司 | Method for refining rutin having content more than or equal to 98% |
| CN115109108A (en) * | 2022-06-21 | 2022-09-27 | 云南八凯农业开发有限公司 | Method for extracting buckwheat rutin |
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| CN104098636B (en) | 2016-07-27 |
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