CN102166249A - Method for extracting active ingredients from honeysuckle leaves - Google Patents
Method for extracting active ingredients from honeysuckle leaves Download PDFInfo
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- CN102166249A CN102166249A CN2011100589597A CN201110058959A CN102166249A CN 102166249 A CN102166249 A CN 102166249A CN 2011100589597 A CN2011100589597 A CN 2011100589597A CN 201110058959 A CN201110058959 A CN 201110058959A CN 102166249 A CN102166249 A CN 102166249A
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 241000205585 Aquilegia canadensis Species 0.000 title claims abstract description 19
- 239000004480 active ingredient Substances 0.000 title abstract 4
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 241000628997 Flos Species 0.000 claims description 22
- 229960004756 ethanol Drugs 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000003463 adsorbent Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 10
- 230000006837 decompression Effects 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000009834 vaporization Methods 0.000 claims description 7
- 230000008016 vaporization Effects 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 abstract description 18
- 230000036541 health Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 235000005985 organic acids Nutrition 0.000 abstract 1
- 238000005728 strengthening Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 5
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- 235000011837 pasties Nutrition 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 4
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 4
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 3
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical group O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 3
- 229940074393 chlorogenic acid Drugs 0.000 description 3
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- 235000001368 chlorogenic acid Nutrition 0.000 description 3
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000341 volatile oil Substances 0.000 description 3
- CWVRJTMFETXNAD-BMNNCGMMSA-N (1s,3r,4s,5r)-3-[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy-1,4,5-trihydroxycyclohexane-1-carboxylic acid Chemical compound O[C@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-BMNNCGMMSA-N 0.000 description 2
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 2
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 2
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 2
- 239000005792 Geraniol Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 229930003944 flavone Natural products 0.000 description 2
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- 229940113087 geraniol Drugs 0.000 description 2
- KRZBCHWVBQOTNZ-DLDRDHNVSA-N isochlorogenic acid Natural products O[C@@H]1[C@H](C[C@@](O)(C[C@H]1OC(=O)C=Cc2ccc(O)c(O)c2)C(=O)O)OC(=O)C=Cc3ccc(O)c(O)c3 KRZBCHWVBQOTNZ-DLDRDHNVSA-N 0.000 description 2
- 229930007744 linalool Natural products 0.000 description 2
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- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
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- 230000003064 anti-oxidating effect Effects 0.000 description 1
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- 244000052616 bacterial pathogen Species 0.000 description 1
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000002024 ethyl acetate extract Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- -1 flavone compound Chemical class 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
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- 230000023597 hemostasis Effects 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for extracting active ingredients from honeysuckle leaves, which comprises the following steps: pretreating fresh honeysuckle leaves; carrying out supercritical CO2 extraction; strengthening and leaching with ultrasonic waves; and concentrating the supernatant liquid to finally obtain the active ingredients. By using the method disclosed by the invention for extracting the active ingredients from the honeysuckle leaves, the content of organic acids can reach more than 50%, thereby greatly improving the application value; and the obtained products can be applied to many occasions such as pharmacy, health products and the like.
Description
Technical field
The present invention relates to a kind of method of from the Chinese crude drug leaf, extracting active component, relate in particular to a kind of method of from leaf of Flos Lonicerae, extracting active component.
Background technology
Flos Lonicerae is a kind of conventional Chinese medicine material, and its main active is chlorogenic acid and isochlorogenic acid, and other active component also have flavonoid, volatilization wet goods, has antibacterial, antiviral, analgesic, antiinflammatory, protects the liver, effects such as hemostasis, antioxidation, immunomodulating.Traditional experience in several thousand and modern age pharmacological evaluation and clinical practice prove that all Flos Lonicerae has stronger antibacterial action and better therapeutic effect for multiple pathogenic bacteria.
In the prior art about the extraction of honey suckle active composition and effective site, only utilize the Flos Lonicerae alabastrum to be raw material, with methanol, ether or ethyl acetate serves as to extract solvent, mainly comprise direct decocting method, infusion process, heat reflow method etc., and various extracting method still are traditional water extract-alcohol precipitation or alcohol extracting-water precipitating, produce a large amount of precipitations in subsequent treatment, not only make chlorogenic acid isoreactivity composition lose in a large number, returning filtration waits technological operation to bring bigger difficulty, time consumption and energy consumption.In addition, it is long that these methods all have extracting cycle, and solvent for use has toxicity, consumption is big, requires the temperature height to cause many shortcomings such as active component degraded, and final objective product extraction ratio and the response rate are very low.Therefore traditional processing technique does not have to make full use of the active component in the Flos Lonicerae, thereby greatly reduces its using value, causes the very big wasting of resources.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes prior art, a kind of method of extracting active component from leaf of Flos Lonicerae is provided, and this method has that technology is simple, cost is low, organic acid content height in easy to operate, the extract, be fit to characteristics such as suitability for industrialized production.
Technical problem of the present invention is realized by following technical scheme:
A kind of method of from leaf of Flos Lonicerae, extracting active component, it carries out as follows:
A. fresh honeysuckle leaf pretreatment: the blade of fresh honeysuckle after 45-60 ℃ of dry 12-17 hour, is ground into 40-300 purpose powder, stored refrigerated, standby;
B. supercritical CO 2 extraction:
Gained powder among the step a is packed in the extraction kettle into 25～35 ℃ of extraction temperature, extracting pressure 20～60 MPa, CO2 flow velocity 10～25 kg/h;
Extract carries out two-stage decompression separation in separating still, the pressure of flash trapping stage still is 10～18 MPa, and temperature is 25～35 ℃; Secondary separating still pressure is 5～8 MPa, and temperature is 25～50 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: step b products therefrom is added 3～10 times extraction solvent by weight, and the intensified by ultrasonic wave extraction temperature is 20～50 ℃, and ultrasonic power is 120～250w, and ultrasonic time is 30～60min; Lixiviating solution-5～0 ℃, with centrifugal 10～20 min of 5000 r/min speed;
The precipitation part adds the extraction solvent of 3～5 times of weight ratios then, repeats above-mentioned steps; Merge the gained supernatant, standby;
D. concentrated supernatant: at 50～60 ℃, reduction vaporization and vacuum drying get paste under the 0.01MPa, and be standby with step c gained supernatant;
E. make active component: steps d gained paste is dissolved with distilled water, the reuse acid for adjusting pH value is 1～7(so that make separated object meet the macroporous resin separation requirement), last macroporous adsorbent resin separates, successively with flow velocity water, the ethanol water eluting of 0.5-1.0ml/min, collect ethanol elution, decompression recycling ethanol, the reuse organic solvent extracts, the reclaim under reduced pressure organic solvent obtains active component at last.
The above-mentioned method of from leaf of Flos Lonicerae, extracting active component, wherein,
Refrigerated storage temperature described in the step a is 0-20 ℃;
Extracting solvent described in the step c is dehydrated alcohol or acetone;
The weight ratio W extractum of distilled water described in the step e and paste: W distilled water=1:10-25; The acid of described adjusting pH value is concentrated hydrochloric acid, and its concentration is 30%-36.5%; Described macroporous adsorbent resin is D101 macroporous adsorbent resin or AB-8 macroporous adsorbent resin; Its volumetric concentration of described ethanol water is 50%～90%; Described organic solvent is ethyl acetate, n-butyl alcohol or isoamyl alcohol.
The present invention proposes the thought that fully utilizes first, as extracting active component raw material, utilizes the technology of the present invention can realize the comprehensive utilization of active component in the leaf of Flos Lonicerae with the Flos Lonicerae blade, expands the using value of Flos Lonicerae plant.Use and contain two big classes in the extractive technique gained active component of the present invention, a class is the liposoluble substance of low pole, as linalool, Flos Lonicerae alcohol, geraniol isoreactivity volatile oil component; Another kind of is strong polar substances such as chlorogenic acid, isochlorogenic acid, flavone compound.Utilize the supercritical CO 2 abstraction technique both can make the high fat-soluble active volatile oil component of added value obtain recycling, be equivalent to again carry out the defat pretreatment for organic acid isoreactivity position in the extraction leaf of Flos Lonicerae, not only help the making full use of of leaf of Flos Lonicerae volatile oil more helped organic acid later stage purification.The method of using macroporous adsorbent resin enrichment, solvent extraction to combine first obtains organic acid content and is higher than 50% extract, has set up the comparatively scientific and reasonable leaf of Flos Lonicerae organic acid extraction and separation process flow process of a cover.This technology has reduced the loss that causes because of precipitation in the conventional leaching process of organic acid, improves the organic acid response rate, makes the total extraction rate reached to 1.0 of organic acid～3.0%; Reduced the difficulty during the conventional extracting solution of organic acid filtered in the later stage; Under the prerequisite that does not influence the organic acid total amount, increased the utilization of linalool, Flos Lonicerae alcohol, geraniol, total flavones etc. in the leaf of Flos Lonicerae.This technology has that technology is simple, cost is low, easy to operate, produce finished product organic acid content advantages of higher, organic acid content is suitable for suitability for industrialized production up to 68%, the gained active component can be used for many occasions such as health product or medicine.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is done step detailed description.
Embodiment 1
A. fresh honeysuckle leaf pretreatment: 500g fresh honeysuckle blade after 14 hours, is ground into 100 purpose powder in 45 ℃ of dryings, cold preservation under 5 ℃ of conditions, standby;
B. supercritical CO 2 extraction:
200g step a gained powder is packed in the extraction kettle into 35 ℃ of extraction temperature, extracting pressure 55 MPa, CO2 flow velocity 15 kg/h; The pressure of flash trapping stage still is 15 MPa, and temperature is 35 ℃, and secondary separating still pressure is 5 MPa, and temperature is 50 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: get 100g step b products therefrom, add the 1000g dehydrated alcohol, temperature is 20 ℃, and ultrasonic power is 200 w, ultrasonic lixiviate 30 min; Lixiviating solution-4 ℃, with centrifugal 20 min of the speed of 5000 r/min;
The precipitation part adds 500 g dehydrated alcohol then, repeats the said extracted step; Merge the gained supernatant, standby;
D. concentrated supernatant: at 50 ℃, 0.01MPa gets pasty masses through reduction vaporization and vacuum drying down, and is standby with step c gained supernatant;
E. make active component: with steps d gained paste 50ml dissolved in distilled water, after the concentrated hydrochloric acid of reuse 30%-36.5% is regulated pH value 1, last D101 macroporous adsorbent resin, flow velocity water, 90% ethanol with 0.5ml/min carries out eluting successively, collect ethanol elution, decompression recycling ethanol, the reuse ethyl acetate extracts, the reclaim under reduced pressure ethyl acetate obtains organic acid content at last and is about 68% active component.
Embodiment 2
A. fresh honeysuckle leaf pretreatment: 500g fresh honeysuckle blade after 12 hours, is ground into 40 purpose powder in 60 ℃ of dryings, cold preservation under 10 ℃ of conditions, standby;
B. supercritical CO 2 extraction:
200g step a gained powder is packed in the extraction kettle into 25 ℃ of extraction temperature, extracting pressure 20 MPa, CO2 flow velocity 10 kg/h; The pressure of flash trapping stage still is 18 MPa, and temperature is 25 ℃, and secondary separating still pressure is 8MPa, and temperature is 25 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: get 100g step b products therefrom, add the 300g dehydrated alcohol, temperature is 50 ℃, and ultrasonic power is 120w, ultrasonic lixiviate 60min; Lixiviating solution-5 ℃, with centrifugal 10 min of the speed of 5000 r/min;
The precipitation part adds the 300g dehydrated alcohol then, repeats the said extracted step; Merge the gained supernatant, standby;
D. concentrated supernatant: at 60 ℃, 0.01MPa gets pasty masses through reduction vaporization and vacuum drying down, and is standby with step c gained supernatant;
E. make active component: with steps d gained paste W extractum: the dissolved in distilled water of W distilled water=1:15, after the concentrated hydrochloric acid of reuse 30%-36.5% is regulated pH value 7, last AB-8 macroporous adsorbent resin, flow velocity water, 50% ethanol with 1.0ml/min carries out eluting successively, collect ethanol elution, decompression recycling ethanol, the reuse n-butyl alcohol extracts, the reclaim under reduced pressure n-butyl alcohol obtains organic acid content at last and is about 60% active component.
Embodiment 3
A. fresh honeysuckle leaf pretreatment: 500g fresh honeysuckle blade after 17 hours, is ground into 300 purpose powder in 50 ℃ of dryings, cold preservation under-20 ℃ of conditions, standby;
B. supercritical CO 2 extraction:
200g step a gained powder is packed in the extraction kettle into 30 ℃ of extraction temperature, extracting pressure 60MPa, CO2 flow velocity 25kg/h; The pressure of flash trapping stage still is 10MPa, and temperature is 30 ℃, and secondary separating still pressure is 6MPa, and temperature is 40 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: get 100g step b products therefrom, add 600g acetone, temperature is 40 ℃, and ultrasonic power is 250w, ultrasonic lixiviate 40min; Lixiviating solution 0 ℃, with the centrifugal 15min of the speed of 5000 r/min;
The precipitation part adds 400g acetone then, repeats the said extracted step; Merge the gained supernatant, standby;
D. concentrated supernatant: at 55 ℃, 0.01MPa gets pasty masses through reduction vaporization and vacuum drying down, and is standby with step c gained supernatant;
E. make active component: with steps d gained paste W extractum: the dissolved in distilled water of W distilled water=1:20, after the concentrated hydrochloric acid of reuse 30%-36.5% is regulated pH value 5, last AB-8 macroporous adsorbent resin, flow velocity water, 80% ethanol with 1.0ml/min carries out eluting successively, collect ethanol elution, decompression recycling ethanol, the reuse isoamyl alcohol extracts, the reclaim under reduced pressure isoamyl alcohol obtains organic acid content at last and is about 62% active component.
Embodiment 4
A. fresh honeysuckle leaf pretreatment: 500g fresh honeysuckle blade after 16 hours, is ground into 200 purpose powder, in 0 ℃ in 55 ℃ of dryings) cold preservation under the condition is standby;
B. supercritical CO 2 extraction:
200g step a gained powder is packed in the extraction kettle into 32 ℃ of extraction temperature, extracting pressure 40MPa, CO2 flow velocity 20kg/h; The pressure of flash trapping stage still is 13MPa, and temperature is 31 ℃, and secondary separating still pressure is 7MPa, and temperature is 35 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: get 100g step b products therefrom, add 800g acetone, temperature is 30 ℃, and ultrasonic power is 150w, ultrasonic lixiviate 50min; Lixiviating solution-3 ℃, with the centrifugal 16min of the speed of 5000 r/min;
The precipitation part adds 300g acetone then, repeats the said extracted step; Merge the gained supernatant, standby;
D. concentrated supernatant: at 60 ℃, 0.01MPa gets pasty masses through reduction vaporization and vacuum drying down, and is standby with step c gained supernatant;
E. make active component: with steps d gained paste W extractum: the dissolved in distilled water of W distilled water=1:15, after the concentrated hydrochloric acid of reuse 30%-36.5% is regulated pH value 3, last AB-8 macroporous adsorbent resin, flow velocity water, 60% ethanol with 1.0ml/min carries out eluting successively, collect ethanol elution, decompression recycling ethanol, the reuse isoamyl alcohol extracts, the reclaim under reduced pressure isoamyl alcohol obtains organic acid content at last and is about 59% active component.
Embodiment 5
A. fresh honeysuckle leaf pretreatment: 500g fresh honeysuckle blade after 14 hours, is ground into 250 purpose powder in 55 ℃ of dryings, cold preservation under 15 ℃ of conditions, standby;
B. supercritical CO 2 extraction:
200g step a gained powder is packed in the extraction kettle into 30 ℃ of extraction temperature, extracting pressure 45MPa, CO2 flow velocity 25kg/h; The pressure of flash trapping stage still is 15MPa, and temperature is 35 ℃, and secondary separating still pressure is 6MPa, and temperature is 45 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: get 100g step b products therefrom, add 700g acetone, temperature is 35 ℃, and ultrasonic power is 250w, ultrasonic lixiviate 45min; Lixiviating solution-1 ℃, with the centrifugal 17min of the speed of 5000 r/min;
The precipitation part adds 400g acetone then, repeats the said extracted step; Merge the gained supernatant, standby;
D. concentrated supernatant: at 60 ℃, 0.01MPa gets pasty masses through reduction vaporization and vacuum drying down, and is standby with step c gained supernatant;
E. make active component: with steps d gained paste W extractum: the dissolved in distilled water of W distilled water=1:15, after the concentrated hydrochloric acid of reuse 30%-36.5% is regulated pH value 3, last D101 macroporous adsorbent resin, flow velocity water, 90% ethanol with 1.0ml/min carries out eluting successively, collect ethanol elution, decompression recycling ethanol, the reuse isoamyl alcohol extracts, the reclaim under reduced pressure isoamyl alcohol obtains organic acid content at last and is about 64% active component.
Claims (4)
1. method of extracting active component from leaf of Flos Lonicerae is characterized in that it carries out as follows:
A. fresh honeysuckle leaf pretreatment: the fresh honeysuckle blade after 45-60 ℃ of dry 12-17 hour, is ground into 40-300 purpose powder, stored refrigerated, standby;
B. supercritical CO 2 extraction:
Gained powder among the step a is packed in the extraction kettle into 25～35 ℃ of extraction temperature, extracting pressure 20～60 MPa, CO2 flow velocity 10～25 kg/h;
Extract carries out two-stage decompression separation in separating still, the pressure of flash trapping stage still is 10～18 MPa, and temperature is 25～35 ℃; Secondary separating still pressure is 5～8 MPa, and temperature is 25～50 ℃, collects product, and is standby;
C. intensified by ultrasonic wave lixiviate: step b products therefrom is added 3～10 times extraction solvent by weight, and the intensified by ultrasonic wave extraction temperature is 20～50 ℃, and ultrasonic power is 120～250w, and ultrasonic time is 30～60min; Lixiviating solution-5～0 ℃, with centrifugal 10～20 min of 5000 r/min speed;
The precipitation part adds the homogeneous solvent of 3～5 times of weight ratios then, repeats above-mentioned steps; Merge the gained supernatant, standby;
D. concentrated supernatant: at 50～60 ℃, reduction vaporization and vacuum drying get paste under the 0.01MPa, and be standby with step c gained supernatant;
E. make active component: steps d gained paste is dissolved with distilled water, behind the reuse acid for adjusting pH value 1～7, last macroporous adsorbent resin, successively with flow velocity water, the ethanol water eluting of 0.5-1.0ml/min, collect ethanol elution, decompression recycling ethanol, the reuse organic solvent extracts, the reclaim under reduced pressure organic solvent obtains active component at last.
2. according to the described method of from leaf of Flos Lonicerae, extracting active component of claim 1, it is characterized in that refrigerated storage temperature is 0-20 ℃ among the described step a; Extracting solvent described in the described step c is dehydrated alcohol or acetone.
3. according to the described method of from leaf of Flos Lonicerae, extracting active component of claim 2, it is characterized in that the weight ratio W extractum of distilled water and paste described in the described step e: W distilled water=1:10-25; The acid of described adjusting pH value is concentrated hydrochloric acid, and its concentration is 30%-36.5%; Its volumetric concentration of described ethanol water is 50%～90%; Described organic solvent is ethyl acetate, n-butyl alcohol or isoamyl alcohol.
4. according to the described method of from leaf of Flos Lonicerae, extracting active component of claim 3, it is characterized in that macroporous adsorbent resin is D101 macroporous adsorbent resin or AB-8 macroporous adsorbent resin among the step e.
Priority Applications (1)
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| CN104382978A (en) * | 2014-10-28 | 2015-03-04 | 广西金昊生物科技有限公司 | Method for extracting effective components of leaves of honeysuckle |
| CN104921289A (en) * | 2015-06-17 | 2015-09-23 | 云南中烟工业有限责任公司 | Honeysuckle glyceryl triacetate extract and application thereof in cigarette |
| CN107684577A (en) * | 2017-10-16 | 2018-02-13 | 孙建忠 | A kind of preparation method of Salvia root P.E |
| CN116270788A (en) * | 2023-02-23 | 2023-06-23 | 济南亿民动物药业有限公司 | Preparation method and application of honeysuckle leaf extract and composition thereof |
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