CN108379315A - A method of extracting bergapten from frutus cnidii - Google Patents
A method of extracting bergapten from frutus cnidii Download PDFInfo
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- CN108379315A CN108379315A CN201810314002.6A CN201810314002A CN108379315A CN 108379315 A CN108379315 A CN 108379315A CN 201810314002 A CN201810314002 A CN 201810314002A CN 108379315 A CN108379315 A CN 108379315A
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- frutus cnidii
- bergapten
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- enzymolysis liquid
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- BGEBZHIAGXMEMV-UHFFFAOYSA-N 5-methoxypsoralen Chemical compound O1C(=O)C=CC2=C1C=C1OC=CC1=C2OC BGEBZHIAGXMEMV-UHFFFAOYSA-N 0.000 title claims abstract description 82
- DBMJZOMNXBSRED-UHFFFAOYSA-N Bergamottin Natural products O1C(=O)C=CC2=C1C=C1OC=CC1=C2OCC=C(C)CCC=C(C)C DBMJZOMNXBSRED-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229960002045 bergapten Drugs 0.000 title claims abstract description 41
- KGZDKFWCIPZMRK-UHFFFAOYSA-N bergapten Natural products COC1C2=C(Cc3ccoc13)C=CC(=O)O2 KGZDKFWCIPZMRK-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 235000019441 ethanol Nutrition 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000003480 eluent Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 9
- 239000002250 absorbent Substances 0.000 claims abstract description 8
- 230000002745 absorbent Effects 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 6
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 5
- 241000212948 Cnidium Species 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 108010059892 Cellulase Proteins 0.000 claims description 13
- 229940106157 cellulase Drugs 0.000 claims description 13
- 238000010828 elution Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000006210 lotion Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 3
- 102000004190 Enzymes Human genes 0.000 claims description 3
- 229940088598 enzyme Drugs 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000284 extract Substances 0.000 description 5
- HPUXDMUGCAWDFW-UHFFFAOYSA-N Osthole Natural products COc1ccc2CCC(=O)Oc2c1C=CC(=O)C HPUXDMUGCAWDFW-UHFFFAOYSA-N 0.000 description 4
- 150000002596 lactones Chemical class 0.000 description 4
- MBRLOUHOWLUMFF-UHFFFAOYSA-N osthole Chemical compound C1=CC(=O)OC2=C(CC=C(C)C)C(OC)=CC=C21 MBRLOUHOWLUMFF-UHFFFAOYSA-N 0.000 description 4
- 241001672694 Citrus reticulata Species 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- OLOOJGVNMBJLLR-UHFFFAOYSA-N imperatorin Chemical compound C1=CC(=O)OC2=C1C=C1C=COC1=C2OCC=C(C)C OLOOJGVNMBJLLR-UHFFFAOYSA-N 0.000 description 3
- XKVWLLRDBHAWBL-UHFFFAOYSA-N imperatorin Natural products CC(=CCOc1c2OCCc2cc3C=CC(=O)Oc13)C XKVWLLRDBHAWBL-UHFFFAOYSA-N 0.000 description 3
- 230000000144 pharmacologic effect Effects 0.000 description 3
- 240000007126 Citrus medica var. sarcodactylis Species 0.000 description 2
- 241000356446 Cnidium monnieri Species 0.000 description 2
- 235000019084 Selinum monnieri Nutrition 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
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- 102100033350 ATP-dependent translocase ABCB1 Human genes 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 241000125183 Crithmum maritimum Species 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 230000010190 G1 phase Effects 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 108010047230 Member 1 Subfamily B ATP Binding Cassette Transporter Proteins 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 244000179970 Monarda didyma Species 0.000 description 1
- 235000010672 Monarda didyma Nutrition 0.000 description 1
- 208000002454 Nasopharyngeal Carcinoma Diseases 0.000 description 1
- 206010061306 Nasopharyngeal cancer Diseases 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 208000008350 Pruritus Vulvae Diseases 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 208000007074 Trichomonas Vaginitis Diseases 0.000 description 1
- 208000025206 Trichomonas vaginitis urogenital infection Diseases 0.000 description 1
- 206010056530 Vulvovaginal pruritus Diseases 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000002137 anti-vascular effect Effects 0.000 description 1
- 239000003908 antipruritic agent Substances 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 206010003246 arthritis Diseases 0.000 description 1
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- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 208000021267 infertility disease Diseases 0.000 description 1
- -1 inflammable Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 201000005202 lung cancer Diseases 0.000 description 1
- 208000020816 lung neoplasm Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 201000011216 nasopharynx carcinoma Diseases 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001582 osteoblastic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 230000002557 soporific effect Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 210000004291 uterus Anatomy 0.000 description 1
- 210000003905 vulva Anatomy 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/234—Cnidium (snowparsley)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The method that the invention discloses a kind of to extract bergapten from frutus cnidii, after pectase mixing is added in pretreated frutus cnidii powder, is added suitable quantity of water, and it is 56 then to adjust pH, stands enzymolysis, obtains enzymolysis liquid A；Enzymolysis liquid A secondary enzymolysis, obtains enzymolysis liquid B；Ethanol in proper amount solution is added in enzymolysis liquid B and obtains supernatant after ultrasonic extraction, centrifugation；Supernatant obtains sample stoste after UF membrane filters；Sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, then elute, and collects eluent B；After eluent B recycling ethyl alcohol, concentrated, drying is to constant weight to get the common cnidium fruit P.E containing bergapten.Present invention process is simple, at low cost, and Extraction solvent used is ethyl alcohol, has no toxic side effect, is suitably applied in large-scale industrial production.
Description
Technical field
It is exactly that one kind extracting Buddhist from frutus cnidii the present invention relates to the Component Extraction field in traditional herbal medicines
The method of hand mandarin orange lactone.
Background technology
Frutus cnidii is the drying and ripening fruit of (Cnidium monnieri (L.) Cuss.) of samphire frutus cnidii cnidium monnieri
It is real.Frutus cnidii is warm-natured, and acrid flavour is bitter, slightly poisonous, has the function of that eliminating dampness wind-dispelling, desinsection be antipruritic, warming kidney and enhancing body, for arthritis with fixed pain caused by dampness waist
Bitterly, impotence due to deficiency of the kidney, uterus cold infertile, control eczema of vulva, married woman's pruritus vulvae, trichomonas vaginitis outside etc..The confirmation of modern age pharmacological research, snake
Osthole is to inhibiting the proliferation of breast cancer cell, the G1 phases being promoted to block and inducing cell apoptosis has obvious effect in machine tool,
In addition there is the effects that reducing blood lipid and antitumor action, inhibition thrombosis, tranquilizing soporific and anti-bacterial, anti-itching.Document report table
Bright, inhibition lung cancer that bergapten has, anti-vascular endothelial cell oxidation, inhibits P glycoprotein, adjusts nasopharyngeal carcinoma cell increment
The effects that saving osteoblastic proliferation and differentiation, it is exactly the same with the effect of Fructus cnidii, there is some evidence that bergapten
One of higher ingredient of content not only in frutus cnidii, multinomial pharmacological research also indicate that it is also frutus cnidii Pharmacological
Main component.
The extraction of bergapten generally uses traditional ethanol refluxing process, this method letter operating time in document report
Long, extraction efficiency is low, and uses a large amount of organic solvents, inflammable, explosive, of high cost, remains in common cnidium fruit P.E obtained
Solvent is unhelpful to health.Therefore currently it is badly in need of that a kind of application method is simple, the non-hazardous bergapten of safety carries
Taking technique.
Invention content
The purpose of the present invention is to provide a kind of application method is simple, safety is non-hazardous to extract bergamot from frutus cnidii
The method of lactone.
Above-mentioned purpose is realized by following scheme：
A method of extracting bergapten from frutus cnidii, which is characterized in that include the following steps：
(1) frutus cnidii is added in the sodium hydroxide solution of a concentration of 0.1-0.2%, stirs evenly, 50-70 DEG C of heating 10-
15 minutes, then heats 15-20 minutes in 125-145 DEG C in autoclave, taken out after pot pressure drop to normal pressure；
(2) material of taking-up is crushed in 70-80 DEG C of heating, drying, crosses 40-60 mesh screens, obtains pretreated frutus cnidii
Powder；
(3) after pectase mixing being added in pretreated frutus cnidii powder, suitable quantity of water is added, it is 5-6 then to adjust pH, is stood
Enzymolysis, obtains enzymolysis liquid A；
(4) cellulase is added in enzymolysis liquid A, tune pH is 5-6, carries out secondary enzymolysis, obtains enzymolysis liquid B；
(5) ethanol in proper amount solution is added in enzymolysis liquid B and obtains supernatant after ultrasonic extraction, centrifugation；
(6) supernatant obtains sample stoste after UF membrane filters；
(7) sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, discards water lotion, then be with volumetric concentration
15~50% ethanol elution discards eluent A, after the ethanol elution for being 60~80% with volumetric concentration, collects eluent B；
(8) by after eluent B recycling ethyl alcohol, concentrated, drying to constant weight is to get the frutus cnidii extraction containing bergapten
Object.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
Step (3) refers to：0.1-0.3 times of pectin for being equivalent to its quality is added in pretreated frutus cnidii powder
Suitable quantity of water is added in enzyme, and tune pH is 5-6, digests 40-60min under conditions of temperature is 40-50 DEG C, obtains enzymolysis liquid A.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
Step (4) refers to：1-2 times of cellulase for being equivalent to cellulase quality is added in enzymolysis liquid A, adjusts pH
For 5-6,100-120min is digested under conditions of temperature is 50-60 DEG C, obtains enzymolysis liquid B.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
Step (5) refers to：The ethanol solution that volume fraction is 30-40% is added in enzymolysis liquid B, is in Extracting temperature
Ultrasonic extraction 3-5 times under conditions of 55-60 DEG C, each 40-70min merge extracting solution, after centrifugation, obtain supernatant, pre-process
Frutus cnidii powder and the volume fraction be 30-40% the solid-liquid ratio of ethanol solution be 0.04-0.1g/mL.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
UF membrane in step (6) uses two-stage purpose ceramic-film filter.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
The king-post diameter of macroporous absorbent resin and pillar height ratio are 1 in the step (7)：8-1：10；
The flow velocity of ethyl alcohol is 1.4-2.5BV/h in the step (7), and sample the amount of stoste described in step (7) is described big
120-150% of the macroporous adsorbent resin to bergapten static saturated adsorption capacity.
A kind of method for extracting bergapten from frutus cnidii, it is characterised in that：
The condition of concentration is in the step (8)：Vacuum degree is -0.1--0.15MPa, temperature is 40-55 DEG C；Dry temperature
Degree is 70-85 DEG C.
Originally anti-bright to have the beneficial effect that：
1, the present invention uses rational pre-treating technology, carries out pre-treatment to frutus cnidii, removes impurity, and can improve
It is rear to use secondary enzymolysis combination ultrasonic extraction and membrane filter method, wherein secondary enzymolysis energy again to the efficiency of the enzymolysis of frutus cnidii
It is enough to distinguish better enzymatic hydrolysis condition to cellulase and pectase so that not interfered with each other when two kinds of enzyme enzymolysis, to more
Thoroughly removal cellulose, starch and colloid etc., are more conducive to the dissolution of bergapten；Two-stage purpose ceramic-film filter can
More thoroughly other interfering substances are filtered, efficient stable.
2, the content of the extract obtained middle bergapten of the present invention greatly improves, and is surveyed through high performance liquid chromatography HPLC
It is fixed, use in the common cnidium fruit P.E obtained by the method for the present invention bergapten content for 10-30% as shown in Figure 1 and Figure 2, and
Bergapten content is less than 0.1% in frutus cnidii before purification.
3, present invention process is simple, at low cost, and Extraction solvent used is ethyl alcohol, is had no toxic side effect, and is suitably applied big
In the production of technical scale metaplasia.
Description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of bergapten, ammidin, Osthole reference substance.Wherein, 1. fingered citron
2. ammidin of mandarin orange lactone, 3. Osthole.
Fig. 2 is the high-efficient liquid phase chromatogram of the frutus cnidii bergapten extract of 1 gained of embodiment.Wherein, 1. fingered citron
2. ammidin of mandarin orange lactone, 3. Osthole.
Specific implementation mode
Embodiment 1, a kind of method for extracting bergapten from frutus cnidii, include the following steps：
(1) frutus cnidii is added in a concentration of 0.1% sodium hydroxide solution, stirs evenly, 60 DEG C heat 15 minutes, then
Heat 20 minutes in 125 DEG C in autoclave, is taken out after pot pressure drop to normal pressure；
(2) material of taking-up is crushed in 70 DEG C of heating, dryings, crosses 40 mesh screens, obtains pretreated frutus cnidii powder；
(3) 0.3 times of pectase for being equivalent to its quality is added in pretreated frutus cnidii powder, suitable quantity of water is added, adjusts
PH is 6, digests 50min under conditions of temperature is 40 DEG C, obtains enzymolysis liquid A.
(4) 1.2 times of cellulase for being equivalent to cellulase quality is added in enzymolysis liquid A, it is 6 to adjust pH, in temperature
120min is digested under conditions of being 50 DEG C, obtains enzymolysis liquid B；
(5) ethanol solution that volume fraction is 30% is added in enzymolysis liquid B, it is super under conditions of Extracting temperature is 60 DEG C
Sound extracts 3 times, each 60min, merges extracting solution, after centrifugation, obtains supernatant, pretreated frutus cnidii powder and the volume point
Number is 0.06g/mL for the solid-liquid ratio of 40% ethanol solution；
(6) after supernatant is using the filtering of two-stage purpose ceramic-film filter UF membrane, sample stoste is obtained；
(7) sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, discards water lotion, then be with volumetric concentration
30% ethanol elution discards eluent A, after the ethanol elution for being 70% with volumetric concentration, collects eluent B；Macroporous absorption
King-post diameter and the pillar height ratio of resin are 1：8, the flow velocity of ethyl alcohol is 1.5BV/h, and the sample the amount of stoste is the macroporous absorption tree
Fat to bergapten static saturated adsorption capacity 150%.
(8) by after eluent B recycling ethyl alcohol, concentrated, drying to constant weight is to get the frutus cnidii extraction containing bergapten
Object, vacuum degree is -0.1MPa, temperature is 45 DEG C；Drying temperature is 75 DEG C.
Embodiment 2, a kind of method for extracting bergapten from frutus cnidii, include the following steps：
(1) frutus cnidii is added in a concentration of 0.2% sodium hydroxide solution, stirs evenly, 50 DEG C heat 15 minutes, then
Heat 15 minutes in 125 DEG C in autoclave, is taken out after pot pressure drop to normal pressure；
(2) material of taking-up is crushed in 80 DEG C of heating, dryings, crosses 40 mesh screens, obtains pretreated frutus cnidii powder；
(3) 0.1 times of pectase for being equivalent to its quality is added in pretreated frutus cnidii powder, suitable quantity of water is added, adjusts
PH is 5.5, digests 50min under conditions of temperature is 50 DEG C, obtains enzymolysis liquid A.
(4) 1.2 times of cellulase for being equivalent to cellulase quality is added in enzymolysis liquid A, it is 5.5 to adjust pH, in temperature
Degree digests 120min under conditions of being 50 DEG C, obtains enzymolysis liquid B；
(5) ethanol solution that volume fraction is 30% is added in enzymolysis liquid B, it is super under conditions of Extracting temperature is 55 DEG C
Sound extracts 5 times, each 60min, merges extracting solution, after centrifugation, obtains supernatant, pretreated frutus cnidii powder and the volume point
Number is 0.06g/mL for the solid-liquid ratio of 40% ethanol solution；
(6) after supernatant is using the filtering of two-stage purpose ceramic-film filter UF membrane, sample stoste is obtained；
(7) sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, discards water lotion, then be with volumetric concentration
25% ethanol elution discards eluent A, after the ethanol elution for being 60% with volumetric concentration, collects eluent B；Macroporous absorption
King-post diameter and the pillar height ratio of resin are 1：8, the flow velocity of ethyl alcohol is 2.5BV/h, and the sample the amount of stoste is the macroporous absorption tree
Fat to bergapten static saturated adsorption capacity 150%.
(8) by after eluent B recycling ethyl alcohol, concentrated, drying to constant weight is to get the frutus cnidii extraction containing bergapten
Object, vacuum degree is -0.1MPa, temperature is 40 DEG C；Drying temperature is 70 DEG C.
Embodiment 3, a kind of method for extracting bergapten from frutus cnidii, include the following steps：
(1) frutus cnidii is added in a concentration of 0.1% sodium hydroxide solution, stirs evenly, 70 DEG C heat 10 minutes, then
Heat 15 minutes in 130 DEG C in autoclave, is taken out after pot pressure drop to normal pressure；
(2) material of taking-up is crushed in 75 DEG C of heating, dryings, crosses 40 mesh screens, obtains pretreated frutus cnidii powder；
(3) 0.2 times of pectase for being equivalent to its quality is added in pretreated frutus cnidii powder, suitable quantity of water is added, adjusts
PH is 6, digests 50min under conditions of temperature is 40 DEG C, obtains enzymolysis liquid A.
(4) 1.5 times of cellulase for being equivalent to cellulase quality is added in enzymolysis liquid A, it is 6 to adjust pH, in temperature
100min is digested under conditions of being 60 DEG C, obtains enzymolysis liquid B；
(5) ethanol solution that volume fraction is 35% is added in enzymolysis liquid B, it is super under conditions of Extracting temperature is 60 DEG C
Sound extracts 4 times, each 40min, merges extracting solution, after centrifugation, obtains supernatant, pretreated frutus cnidii powder and the volume point
Number is 0.06g/mL for the solid-liquid ratio of 40% ethanol solution；
(6) after supernatant is using the filtering of two-stage purpose ceramic-film filter UF membrane, sample stoste is obtained；
(7) sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, discards water lotion, then be with volumetric concentration
40% ethanol elution discards eluent A, after the ethanol elution for being 80% with volumetric concentration, collects eluent B；Macroporous absorption
King-post diameter and the pillar height ratio of resin are 1：8, the flow velocity of ethyl alcohol is 1.8BV/h, and the sample the amount of stoste is the macroporous absorption tree
Fat to bergapten static saturated adsorption capacity 130%.
(8) by after eluent B recycling ethyl alcohol, concentrated, drying to constant weight is to get the frutus cnidii extraction containing bergapten
Object, vacuum degree is -0.15MPa, temperature is 55 DEG C；Drying temperature is 80 DEG C.
Claims (7)
1. a kind of method for extracting bergapten from frutus cnidii, which is characterized in that include the following steps：
(1) frutus cnidii is added in the sodium hydroxide solution of a concentration of 0.1-0.2%, stirs evenly, 50-70 DEG C of 10-15 points of heating
Then clock heats 15-20 minutes in 125-145 DEG C in autoclave, is taken out after pot pressure drop to normal pressure；
(2) material of taking-up is crushed in 70-80 DEG C of heating, drying, crosses 40-60 mesh screens, obtains pretreated frutus cnidii powder；
(3) after pectase mixing being added in pretreated frutus cnidii powder, suitable quantity of water is added, it is 5-6 then to adjust pH, stands enzyme
Solution, obtains enzymolysis liquid A；
(4) cellulase is added in enzymolysis liquid A, tune pH is 5-6, carries out secondary enzymolysis, obtains enzymolysis liquid B；
(5) ethanol in proper amount solution is added in enzymolysis liquid B and obtains supernatant after ultrasonic extraction, centrifugation；
(6) supernatant obtains sample stoste after UF membrane filters；
(7) sample stoste directly crosses macroporous absorbent resin, is first washed with water for several times, discards water lotion, then with volumetric concentration for 15~
50% ethanol elution discards eluent A, after the ethanol elution for being 60~80% with volumetric concentration, collects eluent B；
(8) by after eluent B recycling ethyl alcohol, concentrated, drying is to constant weight to get the common cnidium fruit P.E containing bergapten.
2. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：Step
(3) it refers to：0.1-0.3 times of pectase for being equivalent to its quality is added in pretreated frutus cnidii powder, suitable quantity of water is added,
Tune pH is 5-6, digests 40-60min under conditions of temperature is 40-50 DEG C, obtains enzymolysis liquid A.
3. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：Step
(4) it refers to：1-2 times of cellulase for being equivalent to cellulase quality is added in enzymolysis liquid A, tune pH is 5-6, in temperature
100-120min is digested under conditions of being 50-60 DEG C, obtains enzymolysis liquid B.
4. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：Step
(5) it refers to：The ethanol solution that volume fraction is 30-40%, the item for being 55-60 DEG C in Extracting temperature are added in enzymolysis liquid B
Ultrasonic extraction 3-5 times under part, each 40-70min merge extracting solution, after centrifugation, obtain supernatant, pretreated frutus cnidii powder
The solid-liquid ratio for the ethanol solution for being 30-40% with the volume fraction is 0.04-0.1g/mL.
5. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：Step
(6) UF membrane in uses two-stage purpose ceramic-film filter.
6. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：The step
Suddenly the king-post diameter of macroporous absorbent resin and pillar height ratio are 1 in (7)：8-1：10；
The flow velocity of ethyl alcohol is 1.4-2.5BV/h in the step (7), and sample the amount of stoste described in step (7) is inhaled for the macropore
120-150% of the attached resin to bergapten static saturated adsorption capacity.
7. a kind of method for extracting bergapten from frutus cnidii according to claim 1, it is characterised in that：The step
Suddenly the condition of concentration is in (8)：Vacuum degree is -0.1--0.15MPa, temperature is 40-55 DEG C；Drying temperature is 70-85 DEG C.
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| CN115227751A (en) * | 2022-08-02 | 2022-10-25 | 河北瑞龙生物科技有限公司 | Preparation method of chayote extract |
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| CN115227751A (en) * | 2022-08-02 | 2022-10-25 | 河北瑞龙生物科技有限公司 | Preparation method of chayote extract |
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