CN106726806A - A kind of supercritical extraction method of the effective component extracting from pollen pini - Google Patents
A kind of supercritical extraction method of the effective component extracting from pollen pini Download PDFInfo
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- CN106726806A CN106726806A CN201611056013.6A CN201611056013A CN106726806A CN 106726806 A CN106726806 A CN 106726806A CN 201611056013 A CN201611056013 A CN 201611056013A CN 106726806 A CN106726806 A CN 106726806A
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- pollen pini
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 229930013930 alkaloid Natural products 0.000 claims abstract description 11
- 150000002596 lactones Chemical class 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 239000003814 drug Substances 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- 229930003935 flavonoid Natural products 0.000 claims description 3
- 150000002215 flavonoids Chemical class 0.000 claims description 3
- 235000017173 flavonoids Nutrition 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 229930003944 flavone Natural products 0.000 abstract description 9
- 150000002213 flavones Chemical class 0.000 abstract description 9
- 235000011949 flavones Nutrition 0.000 abstract description 9
- 150000003797 alkaloid derivatives Chemical class 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000003110 anti-inflammatory effect Effects 0.000 abstract description 4
- 230000003020 moisturizing effect Effects 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 3
- 230000003712 anti-aging effect Effects 0.000 abstract description 3
- 150000002632 lipids Chemical class 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- YDNKGFDKKRUKPY-JHOUSYSJSA-N C16 ceramide Natural products CCCCCCCCCCCCCCCC(=O)N[C@@H](CO)[C@H](O)C=CCCCCCCCCCCCCC YDNKGFDKKRUKPY-JHOUSYSJSA-N 0.000 abstract description 2
- CRJGESKKUOMBCT-VQTJNVASSA-N N-acetylsphinganine Chemical compound CCCCCCCCCCCCCCC[C@@H](O)[C@H](CO)NC(C)=O CRJGESKKUOMBCT-VQTJNVASSA-N 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 229940106189 ceramide Drugs 0.000 abstract description 2
- ZVEQCJWYRWKARO-UHFFFAOYSA-N ceramide Natural products CCCCCCCCCCCCCCC(O)C(=O)NC(CO)C(O)C=CCCC=C(C)CCCCCCCCC ZVEQCJWYRWKARO-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 230000005714 functional activity Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- VVGIYYKRAMHVLU-UHFFFAOYSA-N newbouldiamide Natural products CCCCCCCCCCCCCCCCCCCC(O)C(O)C(O)C(CO)NC(=O)CCCCCCCCCCCCCCCCC VVGIYYKRAMHVLU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000037204 skin physiology Effects 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 230000009759 skin aging Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 8
- 239000013558 reference substance Substances 0.000 description 6
- 229930182558 Sterol Natural products 0.000 description 5
- 150000003432 sterols Chemical class 0.000 description 5
- 235000003702 sterols Nutrition 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 3
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 3
- HZYXFRGVBOPPNZ-UHFFFAOYSA-N UNPD88870 Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)=CCC(CC)C(C)C)C1(C)CC2 HZYXFRGVBOPPNZ-UHFFFAOYSA-N 0.000 description 3
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- HCXVJBMSMIARIN-PHZDYDNGSA-N stigmasterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)/C=C/[C@@H](CC)C(C)C)[C@@]1(C)CC2 HCXVJBMSMIARIN-PHZDYDNGSA-N 0.000 description 3
- 229940032091 stigmasterol Drugs 0.000 description 3
- 235000016831 stigmasterol Nutrition 0.000 description 3
- BFDNMXAIBMJLBB-UHFFFAOYSA-N stigmasterol Natural products CCC(C=CC(C)C1CCCC2C3CC=C4CC(O)CCC4(C)C3CCC12C)C(C)C BFDNMXAIBMJLBB-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 description 2
- XVPBINOPNYFXID-JARXUMMXSA-N 85u4c366qs Chemical compound C([C@@H]1CCC[N@+]2(CCC[C@H]3[C@@H]21)[O-])N1[C@@H]3CCCC1=O XVPBINOPNYFXID-JARXUMMXSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 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 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229930015582 oxymatrine Natural products 0.000 description 2
- 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 description 2
- 238000011160 research Methods 0.000 description 2
- 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 description 2
- 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 description 2
- 235000005493 rutin Nutrition 0.000 description 2
- 229960004555 rutoside Drugs 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Substances [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 1
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- -1 sulfoacetic acid mercury Chemical compound 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Dermatology (AREA)
- Engineering & Computer Science (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of supercritical extraction method of the effective component extracting from pollen pini.Lactone component of the present invention can play a part of lipid barrier protection in skin care item, and closely bound up the effects such as with moisturizing anti-inflammatory；Flavones ingredient has the skin care activities such as anti-aging, anti-inflammatory；Composition of alkaloids has the functional structure group similar to ceramide, can play a part of regulation skin physiology function, moisturizing and delay skin aging.The functional activity of three kinds of compositions complements each other, and reaches the purpose of Synergistic, promotes utilization rate of the pollen pini active ingredient in end product.Extracted the present invention relates to three-level, by supercritical extraction technique, in addition to extracting common lactone component, also the two kinds of extractions of more difficult purifying substances of flavones and alkaloid are carried out using residue, the recovery rate of the compositions such as flavones is improve, and then improve the utilization ratio of pollen pini, it is to avoid the wasting of resources, active principle therein is farthest saved simultaneously, bioactivity is improve.
Description
Technical field
Face the invention belongs to pollen pini abstraction technique field, more particularly to a kind of the super of the effective component extracting from pollen pini
Boundary's extracting process.
Background technology
Pollen pini is a kind of pollen kind of dietotherapeutic, and used as Chinese tradition medicinal material, the history of its dietotherapeutic has exceeded
Thousand, with the various health care functions such as promote longevity.Pollen flavones has various beautifying skin-protection functions, there are some researches show it is anti-
Radiation, anti-aging and anti-oxidant aspect have good performance.
The extraction and separation process of current pollen pini mostly concentrates on water extraction and alcohol extraction process research, to the esters in pollen pini
Composition and composition of alkaloids are difficult to reach the purpose for isolating and purifying；Abstraction technique is waited to be typically for pollen pini using overcritical
In lactone component such as sterol, glyceric acid etc., but active component to being related under traditional extraction technique is rare to be related to, therefore very
The difficult active ingredient farthest utilized in pollen pini.
The content of the invention
The deficiency that the present invention exists for above-mentioned prior art, there is provided a kind of the super of the effective component extracting from pollen pini faces
Boundary's extracting process.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of the super of the effective component extracting from pollen pini faces
Boundary's extracting process, comprises the following steps：
(1) total lactone component is extracted：To be fitted into extractor by the pollen pini of dry, broken wall and sterilizing, be in temperature
40-50 DEG C, pressure be 25MPa, CO2Flow velocity is 25L/h-35L/h, under the conditions of continuous extraction 2h；With extracting fats
The CO of compound2Fluid enter separation reactor I in, temperature be 40 DEG C -60 DEG C, pressure be 8MPa under the conditions of carry out one-level separation；Again
Into in separation reactor I I, temperature be 30 DEG C, pressure be 6MPa under the conditions of carry out the second-order separation；
(2) total flavonoid composition is extracted：The medicine residue that step (1) is obtained pressure be 20-40MPa, temperature be 60-
80℃、CO2Flow velocity be 25L/h-35L/h under conditions of extract 1.5h；
(3) extract total alkaloids composition：The medicine residue that step (2) is obtained is the ammonia of 10-20% with 100mL, concentration
The aqueous solution mix, alkalization 1-2h after, temperature be 70 DEG C, pressure be 40MPa, CO2Flow velocity is extraction under conditions of 35-45L/h
1.5h；
(4) extraction component of step (1) (2) (3) is mixed.
Wherein, the ethanol that 200-400ml, concentration are 80-90% is added in the extraction process of step (2) as entrainment reagent.
300ml absolute ethyl alcohols are added in extraction process in step (3) as entrainment reagent.
CO described in step (1) (2) (3)2Purity is more than 99%.
The beneficial effects of the invention are as follows：
1st, the lactone component that the present invention is extracted can play a part of lipid barrier protection, and same moisturizing in skin care item
The effects such as anti-inflammatory, is closely bound up；The flavones ingredient of extraction has the skin care activities such as anti-aging, anti-inflammatory；The alkaloids of extraction
Composition has the functional structure group similar to ceramide, can play regulation skin physiology function, moisturizing and delaying skin
The effect of aging.The functional activity of three kinds of compositions complements each other, and reaches the purpose of Synergistic, promotes pollen pini active ingredient to exist
Utilization rate in end product.
2nd, existing pollen pini ultrasonic extraction is generally that one-level is extracted, mainly for fatty constituents therein, or lipid
Synthesis precursor substance phytosterin compound.The material that the present invention is extracted is total esters, except common fats or sterols
Composition, also including phosphatide constituents and volatile oil composition etc..Moreover, it relates to three-level is extracted, by supercritical extract
Technology, in addition to extracting common lactone component, also carries out carrying for flavones and two kinds of more difficult purifying substances of alkaloid using residue
Take, improve the recovery rate of the compositions such as flavones, and then improve the utilization ratio of pollen pini, it is to avoid the wasting of resources, while most
Big degree saves active principle therein, improves bioactivity.
Specific embodiment
Principle of the invention and feature are described below in conjunction with example, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment 1
A kind of supercritical extraction method of the effective component extracting from pollen pini, comprises the following steps：
(1) total lactone component is extracted：Pollen pini is fitted into extractor, temperature be 40-50 DEG C, pressure be 25MPa,
CO2Flow velocity is continuous extraction 2h under the conditions of 30L/h；With the CO for extracting fat compound2Fluid enters in separation reactor I,
Temperature be 50 DEG C, pressure be 8MPa under the conditions of carry out one-level separation；In entering back into separation reactor I I, temperature be 30 DEG C, pressure be
The second-order separation is carried out under the conditions of 6MPa；
(2) total flavonoid composition is extracted：The medicine residue that step (1) is obtained pressure be 20-40MPa, temperature be 70
℃、CO2Flow velocity be 30L/h under conditions of extract 1.5h, extraction process in add 200-400ml, concentration for 80-90% second
Alcohol is used as entrainment reagent；
(3) extract total alkaloids composition：The medicine residue that step (2) is obtained is the ammonia of 10-20% with 100mL, concentration
The aqueous solution mix, alkalization 1-2h after, temperature be 70 DEG C, pressure be 40MPa, CO2Flow velocity is extraction under conditions of 40L/h
1.5h, adds 300ml absolute ethyl alcohols as entrainment reagent in extraction process；
(4) extraction component of step (1) (2) (3) is mixed.
The assay of each extract component：
1st, total sterol content is determined
The preparation of reference substance titer：Precision weighs stigmasterol reference substance 0.022g, and 50mL is dissolved and be settled to methyl alcohol
Volumetric flask is used as reference substance standard liquid.
The preparation of developer：0.5g mercury oxide is weighed, precision adds the 2mL concentrated sulfuric acids and 10mL distilled water, ultrasonic dissolution, amount
Take the 1mL solution to be placed in 100mL volumetric flasks, scale is settled to glacial acetic acid and concentrated sulfuric acid mixed solution (1: 2).
The preparation of need testing solution：Precision weighs solution after the extraction of 0.5g one-levels, is dissolved with methyl alcohol and quantified to 10mL and held
Measuring bottle is used as need testing solution.
Assay method：Take need testing solution 2mL and be placed in 10mL volumetric flasks and be settled to scale with sulfoacetic acid mercury reagent,
At 410nm wavelength, with methyl alcohol as its absorbance of blank determination.
Linearity and range：Precision draws stigmasterol standard solution 1.0,2.0,4.0,6.0,10.0mL and is respectively placed in 10mL
In volumetric flask and with methanol constant volume to scale, as reference substance solution.Its absorbance is determined at 410nm wavelength, it is dense with stigmasterol
Degree (C) is abscissa, and absorbance (A) makees regression curve, obtains regression equation for ordinate.
Experimental result:Sterol content is 31.69mg/mL during result measures solution, is carried with the same yield of traditional solvent extraction
Take sterol content only 10.19mg/mL. in liquid
2nd, flavones content is determined:
Absorption maximum peak position determines：Accurate rutin standard liquid (0.55g/L) 10mL that draws is used in 50ml volumetric flasks
30% ethanol is mended to 25mL, adds 1.4mL, 5%NaNO2Shake up, 1.4mL, 10%Al (NO are added after placing 5min3)3, 6min
After add 10mL, 1mol/L NaOH mixings, be diluted to scale with 30% ethanol, determine its λ max after 10min, reference is sky
White reagent.
The drafting of standard curve：Above-mentioned rutin standard liquid 1mL, 2mL, 4mL, 6mL, 8mL, 10mL is taken respectively in 6
In 50mL volumetric flasks, mended to 25mL with 30% ethanol, add 1.4mL, 5%NaNO2Shake up, place 5min after add 1.4mL,
10%Al (NO3)3, 10mL, 1mol/L NaOH are added after 6min, mix, it is diluted to scale with 30% ethanol.In wavelength
Light absorption value is determined at 510nm, reference is blank reagent.
The measure of sample solution：1mL extract solutions are taken, 12.5mL is supplemented to 30% alcohol-water in 25mL volumetric flasks, plus
Enter 0.7mL natrium nitrosums, shake up, 0.7mL, l0%Al (NO are added after placing 5min3)3, add people 5mL, 1mol/L after 6min again
NaOH is mixed, and scale is diluted to 30% ethanol, and its absorbance under 510nm wavelength is determined after 10min, and reference is tried for blank
Agent.
Experimental result：Flavones content is 2.38mg/mL in measuring extract solution.
3rd, alkaloid content determination：
The drafting of standard curve：Accurately measured with pipette oxymatrine reference substance solution 1mL, 2mL, 3mL, 4mL,
5mL, 6mL, are placed in dry conical flask with stopper, respectively add distilled water to 6mL, divide and take 5mL, are separately added into the buffer solution of pH value 7.0
5mL, then the accurate addition bromothymol blue titer 2.0mL of concentration 0.025% and chloroform 10.0mL successively, shake 1min, turn
Move to 50mL separatory funnels and place layering, stand 1h, divide and take chloroform layer, the mensuration absorbance at 417nm wavelength.
The another chloroform operated (be not added with oxymatrine reference substance solution) with same method is as blank.
With concentration (C) as abscissa, absorbance (A) is ordinate, draws standard curve.
Sample determination：Take respectively during dilution 5.0mL puts separatory funnel, sequentially add the cushioning liquid 5mL of pH value 7.0, dense
0.025% bromothymol blue titer 2.0mL and chloroform 10.0mL is spent, 1min is shaken, 1h is stood, is divided and is taken chloroform layer.With purple
Outer visible spectrophotometer mensuration absorbance at 417nm wavelength.The absorbance that will be measured substitutes into regression equation, calculates and extracts
The content of TA in liquid.
Experimental result：Alkaloid is 1.94mg/mL in extract solution.If not using supercritical extract, can only use has
Machine solvent is enriched with to alkaloid, influences product later-stage utilization.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (4)
1. a kind of supercritical extraction method of the effective component extracting from pollen pini, it is characterised in that comprise the following steps：
(1) total lactone component is extracted：To be fitted into extractor by the pollen pini of dry, broken wall and sterilizing, be 40-50 in temperature
DEG C, pressure be 25MPa, CO2Flow velocity is 25L/h-35L/h, under the conditions of continuous extraction 2h；With extracting fat compound
CO2Fluid enter separation reactor I in, temperature be 40 DEG C -60 DEG C, pressure be 8MPa under the conditions of carry out one-level separation；Enter back into point
In kettle II, temperature be 30 DEG C, pressure be 6MPa under the conditions of carry out the second-order separation；
(2) total flavonoid composition is extracted：The medicine residue that step (1) is obtained pressure be 20-40MPa, temperature be 60-80
℃、CO2Flow velocity be 25L/h-35L/h under conditions of extract 1.5h；
(3) extract total alkaloids composition：The medicine residue that step (2) is obtained is with 100mL, concentration for the ammoniacal liquor of 10-20% is molten
Liquid mix, alkalization 1-2h after, temperature be 70 DEG C, pressure be 40MPa, CO2Flow velocity be 35-45L/h under conditions of extract 1.5h；
(4) extraction component of step (1) (2) (3) is mixed.
2. supercritical extraction method according to claim 1, it is characterised in that added in the extraction process of step (2)
200-400ml, concentration are the ethanol of 80-90% as entrainment reagent.
3. supercritical extraction method according to claim 1, it is characterised in that added in the extraction process in step (3)
300ml absolute ethyl alcohols are used as entrainment reagent.
4. supercritical extraction method according to claim 1, it is characterised in that the CO described in step (1) (2) (3)2It is pure
Spend is more than 99%.
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| CN108498550A (en) * | 2018-03-07 | 2018-09-07 | 浙江亚林生物科技股份有限公司 | The preparation method of uranidin in a kind of extraction pollen pini |
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