CN108057045A - A kind of CO2The method of means of supercritical extraction agar polyphenol and its agar polyphenol purposes - Google Patents
A kind of CO2The method of means of supercritical extraction agar polyphenol and its agar polyphenol purposes Download PDFInfo
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- CN108057045A CN108057045A CN201810143632.1A CN201810143632A CN108057045A CN 108057045 A CN108057045 A CN 108057045A CN 201810143632 A CN201810143632 A CN 201810143632A CN 108057045 A CN108057045 A CN 108057045A
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- agar
- polyphenol
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- supercritical extraction
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- 229920001817 Agar Polymers 0.000 title claims abstract description 130
- 239000008272 agar Substances 0.000 title claims abstract description 115
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 109
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 76
- 239000000284 extract Substances 0.000 claims abstract description 29
- 230000000694 effects Effects 0.000 claims abstract description 16
- 102000004139 alpha-Amylases Human genes 0.000 claims abstract description 8
- 108090000637 alpha-Amylases Proteins 0.000 claims abstract description 8
- 229940024171 alpha-amylase Drugs 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 6
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 67
- 235000019441 ethanol Nutrition 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000741 silica gel Substances 0.000 claims description 19
- 229910002027 silica gel Inorganic materials 0.000 claims description 19
- 102100024295 Maltase-glucoamylase Human genes 0.000 claims description 8
- 108010028144 alpha-Glucosidases Proteins 0.000 claims description 8
- 239000008280 blood Substances 0.000 claims description 8
- 210000004369 blood Anatomy 0.000 claims description 8
- 230000002401 inhibitory effect Effects 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 230000036541 health Effects 0.000 abstract description 6
- 235000013305 food Nutrition 0.000 abstract description 5
- 238000004108 freeze drying Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 231100001261 hazardous Toxicity 0.000 abstract description 2
- 239000003472 antidiabetic agent Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 235000010419 agar Nutrition 0.000 description 103
- 239000000287 crude extract Substances 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 14
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 12
- 239000003814 drug Substances 0.000 description 7
- 239000003480 eluent Substances 0.000 description 6
- 229940074391 gallic acid Drugs 0.000 description 6
- 235000004515 gallic acid Nutrition 0.000 description 6
- 229940079593 drug Drugs 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 235000006708 antioxidants Nutrition 0.000 description 4
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 4
- 230000007760 free radical scavenging Effects 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 235000011299 Brassica oleracea var botrytis Nutrition 0.000 description 3
- 240000003259 Brassica oleracea var. botrytis Species 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LWFUFLREGJMOIZ-UHFFFAOYSA-N 3,5-dinitrosalicylic acid Chemical class OC(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O LWFUFLREGJMOIZ-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 206010020772 Hypertension Diseases 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 230000009102 absorption Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003392 amylase inhibitor Substances 0.000 description 2
- 230000003466 anti-cipated effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 235000019628 coolness Nutrition 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229940088598 enzyme Drugs 0.000 description 2
- 230000002218 hypoglycaemic effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000028161 membrane depolarization Effects 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 101710171801 Alpha-amylase inhibitor Proteins 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000206650 Gelidiaceae Species 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 241000003857 Parmelia saxatilis Species 0.000 description 1
- 230000002292 Radical scavenging effect Effects 0.000 description 1
- 241000206572 Rhodophyta Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 239000003888 alpha glucosidase inhibitor Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003276 anti-hypertensive effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000009412 basement excavation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 1
- 231100000673 dose–response relationship Toxicity 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000021384 green leafy vegetables Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 230000001631 hypertensive effect Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012476 oxidizable substance Substances 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- -1 sulfuric acid ester Chemical class 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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
- A61K36/02—Algae
- A61K36/04—Rhodophycota or rhodophyta (red algae), e.g. Porphyra
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- 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
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- 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
Abstract
The present invention discloses a kind of CO of agar polyphenol2Supercritical extraction method and its agar polyphenol purposes, specifically, the invention discloses a kind of CO of agar polyphenol extract2Supercritical extraction method comprises the following steps：Specifically include cleaning, vacuum drying, crushing, CO2Supercritical extract, macroreticular resin purification and freeze-drying step.The CO of the agar polyphenol2Supercritical extraction process is easy to operate, selectivity is good, the polyphenol product purity without hazardous solvent residual, extraction efficiency height, extraction is high, can be effectively prevented the oxidation of agar polyphenol component, CO2Supercritical extract is a kind of method of suitable extraction health care agar polyphenol.Agar polyphenol extract, available for preparing antioxidant, it can also be used to inhibit α glucuroides and alpha amylase activity, can be applied in hypoglycemic drug, health products and food.
Description
Technical field
The present invention relates to seaweed products deep-processing and colligating-using fields.More particularly to a kind of CO2Means of supercritical extraction parmelia saxatilis
The method of dish polyphenol and its agar polyphenol purposes.
Background technology
Agar is Rhodophyta Gelidiaceae also known as Chinese little greens, ox horn dish, freezes dish etc., with being distributed widely in China coast
Area.Agar mainly contains a variety of chemical compositions such as phenols, flavonoids, polysaccharide, minerals, stone as a kind of Medicinal Algae
The clearing lung and eliminating phlegm of cauliflower energy, heat-clearing and damp-drying drug, nourishing yin and lessening fire, cooling blood and hemostasis, and have relieving summer-heat effect.Alginate especially contained by it
Class substance has antihypertensive effect, and contained starch sulfuric acid ester is polysaccharose substance, has lipid-reducing function, to hypertension, high blood
Fat has certain preventive and therapeutic effect.Also containing abundant dietary fiber in agar.
Modern medicine study shows that polyphenol is particularly suitable for hypertensive patient or hyperlipidemia patient, has significantly drop
Pressure, effect for reducing fat, are known as being " natural depressor ", while it also has anti-oxidant, hypoglycemic, anticancer, antibacterial, removing freely
The multiple efficacies such as base.Therefore, polyphenol has become the hot spot studied, developed in recent years, in medicine, food, cosmetics, health care
The fields such as product have broad application prospects.
At present, terrestrial plant is mostly focused on for the research of polyphenol, the extraction of terrestrial plant polyphenol mainly has solvent to carry
Take, microwave radiation exaraction, ultrasound assisted extraction, supercritical extract the methods of.Solvent extraction method often introduces some to people
The unfavorable harmful components residual of body is wherein.Supercritical CO2Abstraction technique has technique letter as a kind of new extractive technique
The advantages such as single, selectivity is good, no solvent residue, extraction efficiency height, product purity height, particularly suitable for thermal sensitivity and readily oxidizable substance
The extraction of matter is widely used in the extraction of terrestrial plant polyphenol.But polyphenol molecular polarity is big, in CO2Fluid
In solubility it is smaller, direct extraction yield it is not high, it is necessary to by add ethyl alcohol isopolarity entrainer increase to aldehydes matter
Solvability, so as to improve effect of extracting, and the extraction of seeweed polyphenol and comprehensive utilization are rarely reported, and especially some red algaes are planted
Interior of articles meets the characteristics of hydro-thermal melts condensation rich in the algal polysaccharides such as agar, agar etc. so that this kind of seeweed polyphenol is in extraction side
It is limited in method, extraction efficiency is not high.To realize the utilization to agar polyphenol, it is necessary to further widen agar polyphenol
Research field, in high-new extractive technique apply and bioactivity excavate etc. make a breakthrough.
The content of the invention
In view of the above-mentioned problems, one object of the present invention provides a kind of CO2The method of means of supercritical extraction agar polyphenol, drop
In low agar active ingredient agar polyphenol extraction process degree of oxidation, so as to improve the extraction of agar polyphenol effect
Rate, invention also provides the purposes of agar polyphenol extract prepared by the above method, are preparing the application of antioxidant, use
In inhibition alpha-glucosidase and alpha-amylase activity (that is, answering in alpha-glucosidase and alpha-amylase inhibitor is prepared
With), prepare the application contributed in the drug, health products and food that reduce blood glucose.
Technical solution provided by the invention is：
A kind of CO2The method of means of supercritical extraction agar polyphenol, comprises the following steps：
Step 1 cleans up agar, is placed into vacuum drying chamber and is dried in vacuo at 30~60 DEG C, makes wherein water
Divide and drop to less than 5%；
Step 2 crushes dried agar, is sieved with 40~60 mesh sieve；
Step 3 by the silica gel of 200~300 mesh of the quality such as the agar powder addition after sieving, is packed into extraction kettle,
CO2Supercritical extract, fluid extraction pressure are 10~40MPa, and 35~70 DEG C of extraction temperature, 75% ethyl alcohol does entrainer, presss from both sides
Band agent flow velocity is 1~6mL/min, and extraction time is l~3h, obtains agar polyphenol.
Preferably, further include：Step 3 is obtained agar polyphenol to carry through macroreticular resin D-101 progress essence, then is eluted,
Rotary evaporation removes ethyl alcohol at room temperature, when then freeze-drying 8~16 is small, obtains faint yellow powdery agar polyphenol.
Preferably, supercritical extract pressure is 20MPa in step 3, extraction temperature is 60 DEG C, the stream of entrainer ethyl alcohol
Speed is 1.5mL/min, extraction time 2h.
Preferably, fluid extraction pressure is 20MPa in step 3.
Preferably, extraction temperature is 60 DEG C in step 3.
Preferably, extraction time is 2h in step 3.
It is a kind of to utilize the CO2The use for the agar polyphenol that the method for means of supercritical extraction agar polyphenol is extracted
On the way, for inhibiting the activity of alpha-glucosidase and/or α-amylase.
It is a kind of to utilize the CO2The agar polyphenol that the method for means of supercritical extraction agar polyphenol is extracted is reducing
Application in blood glucose.
It is a kind of to utilize the CO2The use for the agar polyphenol that the method for means of supercritical extraction agar polyphenol is extracted
On the way, it is used to prepare antioxidant.
Beneficial effects of the present invention are as follows：
Firstth, a kind of agar polyphenol CO is provided2The new method of means of supercritical extraction, sample extraction is before plus silica gel is mixed thoroughly
It can effectively prevent the agar polysaccharide component during supercritical extract from dissolving out in extraction process gas circuit is caused to block phenomenon, make
Obtain CO2This method of means of supercritical extraction agar polyphenol can be carried out efficiently, significantly improve CO2Means of supercritical extraction agar is more
The extraction efficiency of phenol；
Secondth, CO is passed through2Supercritical extraction technique realizes the high efficiency extraction of agar polyphenol, and operating procedure is easy, choosing
Selecting property is good, high without hazardous solvent residual, extraction efficiency height, product purity；
3rd, the extracting method that the present invention uses is completed under relatively low temperature, and condition is milder, is neither influenced more
The extraction effect of phenols component, and be conducive to being stabilized for polyphenol components, polyphenol is effectively prevented in extraction process
Oxidation deterioration；
4th, in conclusion the present invention provides a kind of operating procedure simplicity, can effectively prevent seeweed polyphenol oxidation deterioration
Method, to realizing utilization to agar polyphenol, widen agar polyphenol and applied in high-new extractive technique and biology
The research field of activity excavation etc., develops into the health food of assistant hypoglycemic or the potentiality of drug, there is very big exploitation value
Value.
Description of the drawings
Fig. 1 is influence figure of the embodiment 1-5 extracting pressures to agar polyphenol recovery rate；
Fig. 2 is influence figure of the embodiment 6-10 extraction temperatures to agar polyphenol recovery rate；
Fig. 3 is influence figure of the embodiment 11-15 extraction times to agar polyphenol recovery rate；
Fig. 4 is that the agar total polyphenols that present invention extraction obtains are measured knot with gallic acid and the total reducing power of Vc progress
Fruit is schemed；
Fig. 5 is that the agar total polyphenols that present invention extraction obtains carry out DPPH free radical scavenging activity surveys with gallic acid and Vc
Determine experimental result picture.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, those skilled in the art's reference to be made to say
Bright book word can be implemented according to this.
A kind of CO2The method of means of supercritical extraction agar polyphenol, specifically includes following steps：
Step 1) cleans fresh agar, drains, and is subsequently placed in vacuum drying chamber and is dried under vacuum at 50 DEG C
Agar moisture is less than 5%.When freezing 2 is small under the conditions of -35 DEG C of refrigerator of placement after Vacuum Package, medicinal herb grinder is then used
It crushes, is crushed to 20~60 mesh, crushing process ensures that temperature is not higher than 40 DEG C；
Agar powder after crushing is placed in the sieve of 40~60 mesh and sieves by step 2), the agar powder after sieving
It is preserved for use as being placed in the brown drier of drier；
Step 3) weighs a certain amount of agar powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI
In the extraction kettle of supercritical extract instrument (SFE-2), CO is carried out2Supercritical extract, fluid extraction pressure are 10~30MPa, are extracted
35~70 DEG C of temperature, 75% ethyl alcohol do entrainer, and entrainer flow velocity is 1~6mL/min, and extraction time is l~3h, obtains stone
Cauliflower polyphenol crude extract；
Agar polyphenol crude extract obtained by step (3) is added to the D-101 type macroporous absorptions anticipated by step 4)
Resin column is eluted with distilled water, the low-concentration ethanol not higher than 15%, water or low-concentration ethanol eluent is discarded not successively
With, except the big impurity of depolarization, then with 80% ethanol solution elute, collect eluent；
Eluent collected by step (4) is placed in the distillation bottle of Rotary Evaporators by step 5), and rotation at room temperature is steamed
Hair concentration removes ethyl alcohol, obtains the suspended matter aqueous solution of agar polyphenol, put -80 DEG C of refrigerator deep coolings 2 it is small when, it is then dry with freezing
When dry device freeze-drying 8~16 is small, faint yellow powdery agar polyphenol is obtained；
Step 6) assay method：Agar Determination of Polyphenols is carried out by forint phenol (Folin-Ci DEG C of alteus) colorimetric method
Measure；The external anti-of agar polyphenol is evaluated by measure to total reducing power, DPPH free radical scavenging activities determination experiment
Oxidation activity；Agar polyphenol is measured to alpha-glucosaccharase for substrate with p-nitrophenyl-α-D- glucopyranosides (PNPG)
The inhibitory action of enzyme measures inhibition of the agar polyphenol to alpha-amylase activity with 3,5- dinitrosalicylic acids (DNS) for substrate
Effect；
The agar polyphenol extract of the present invention has preferable inoxidizability and inhibits alpha-glucosidase and alphalise starch
The bioactivity of enzyme activity, therefore, available for preparing antioxidant and with alpha-glucosidase and alpha-amylase inhibition
Drug, health products and food, that is, preparing helps to reduce the application in the drug of blood glucose, health products and food.
Embodiment 1：
A kind of CO2The method of means of supercritical extraction agar polyphenol, specifically includes following steps：
Step 1) cleans fresh agar, drains, and is subsequently placed in vacuum drying chamber and is dried under vacuum at 50 DEG C
Agar moisture is less than 5%.When freezing 2 is small under the conditions of -35 DEG C of refrigerator of placement after Vacuum Package, medicinal herb grinder is then used
It crushes, is crushed to 20~60 mesh, crushing process ensures that temperature is not higher than 40 DEG C；
Agar powder after crushing is placed in the sieve of 40~60 mesh and sieves by step 2), the agar powder after sieving
It is preserved for use as being placed in the brown drier of drier；
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In the extraction kettle of critical abstraction instrument, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% second
Alcohol does entrainer, and entrainer flow velocity is 1.5mL/min, extraction time 2h, obtains agar polyphenol crude extract；
Agar polyphenol crude extract obtained by step (3) is added to the D-101 type macroporous absorptions anticipated by step 4)
Resin column is eluted with distilled water, the low-concentration ethanol not higher than 15%, water or low-concentration ethanol eluent is discarded not successively
With, except the big impurity of depolarization, then with 80% ethanol solution elute, collect eluent；
Eluent collected by step (4) is placed in the distillation bottle of Rotary Evaporators by step 5), and rotation at room temperature is steamed
Hair concentration removes ethyl alcohol, obtains the suspended matter aqueous solution of agar polyphenol, put -80 DEG C of refrigerator deep coolings 2 it is small when, it is then dry with freezing
When dry device freeze-drying 16 is small, faint yellow powdery agar polyphenol is obtained.
Embodiment 2：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In the kettle of critical abstraction instrument, CO is carried out2Supercritical extract, extracting pressure 10MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol is done
Entrainer, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 3：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 15MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 4：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO2 supercritical extracts are carried out, extracting pressure 25MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 5：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO2 supercritical extracts are carried out, extracting pressure 30MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 6：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 35 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 7：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 40 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 8：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 50 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 9：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 10：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 70 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 11：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 0.5h, obtain agar polyphenol crude extract.
Embodiment 12：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 1h, obtain agar polyphenol crude extract.
Embodiment 13：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 1.5h, obtain agar polyphenol crude extract.
Embodiment 14：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2h, obtain agar polyphenol crude extract.
Embodiment 15：[step 1), 2), 4), 5) and, 6) with embodiment 1]
Step 3) weighs 3.0000g agars powder and the silica gel of 200~300 mesh of equivalent is uniformly mixed, and is placed in ASI and surpasses
In critical abstraction instrument kettle, CO is carried out2Supercritical extract, extracting pressure 20MPa, 60 DEG C of extraction temperature, 75% ethyl alcohol presss from both sides
Band agent, entrainer flow velocity are 1.5mL/min, extraction time 2.5h, obtain agar polyphenol crude extract.
Agar Determination of Polyphenols is obtained to embodiment 1-15 using forint phenol (Folin-Ci DEG C of alteus) colorimetric method
It measures, as a result as shown in Figure 1 to Figure 3；
The agar total polyphenols that present invention extraction obtains are carried out total reducing power with gallic acid and Vc to be measured, it is each total
The measurement result of reducing power is as shown in figure 4, in the range of agar polyphenol concentration is from 0.005mg/mL to 0.045mg/mL, stone
The reducing power of cauliflower polyphenol increases as polyphenol concentration increases, in dose dependent.When polyphenol concentration is at the highest notch
When (0.045mg/mL), the light absorption value of reducing power has reached comparable sodium gallic acid and Vc reducing power light absorption values
47.60%th, 48.67%, it was demonstrated that agar polyphenol has certain reducing power；
The agar total polyphenols that present invention extraction obtains and gallic acid and Vc are subjected to DPPH free radical scavenging activity measure
Test to evaluate the antioxidation activity in vitro of agar polyphenol, test result as figure 5 illustrates, with the mass concentration of agar polyphenol
Increase, DPPH free radical scavenging activities are also with rising, when mass concentration reaches maximum 0.045mg/mL, Scavenging activity
It is 74.48%, 72.58% of gallic acid and Vc under homogenous quantities concentration conditions, it is certain that this illustrates that agar polyphenol has
DPPH radical scavenging activities.
Agar polyphenol is measured to alpha-glucosidase for substrate with p-nitrophenyl-α-D- glucopyranosides (PNPG)
Inhibitory action, the results show agar polyphenol has inhibitory action to alpha-glucosidase, with 3,5- dinitrosalicylic acids (DNS)
Agar polyphenol is measured to the inhibitory action of alpha-amylase activity for substrate, and the results show agar polyphenol is to alpha-amylase activity
There is inhibitory action, the similary agar total polyphenols obtained using present invention extraction are applied to the high crowd of blood glucose, and having reduces blood
The function of sugar.
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, it is of the invention and unlimited
In specific details and shown here as the embodiment with description.
Claims (9)
1. a kind of CO2The method of means of supercritical extraction agar polyphenol, which is characterized in that comprise the following steps：
Step 1 cleans up agar, is placed into vacuum drying chamber and is dried in vacuo at 30~60 DEG C, makes wherein moisture drop
To less than 5%；
Step 2 crushes dried agar, is sieved with 40~60 mesh sieve；
Step 3 by the silica gel of 200~300 mesh of the quality such as the agar powder addition after sieving, is packed into extraction kettle, CO2It is super to face
Boundary extracts, and fluid extraction pressure is 10~40MPa, and 35~70 DEG C of extraction temperature, 75% ethyl alcohol does entrainer, entrainer flow velocity
For 1~6mL/min, extraction time is l~3h, obtains agar polyphenol.
2. CO as described in claim 12The method of means of supercritical extraction agar polyphenol, which is characterized in that further include：By step
Three obtain agar polyphenol carries through macroreticular resin D-101 progress essence, then elutes, and rotary evaporation removes ethyl alcohol, Ran Houleng at room temperature
It is lyophilized it is dry 8~16 it is small when, obtain faint yellow powdery agar polyphenol.
3. CO as claimed in claim 22The method of means of supercritical extraction agar polyphenol, which is characterized in that overcritical in step 3
Extracting pressure is 20MPa, extraction temperature is 60 DEG C, the flow velocity of entrainer ethyl alcohol is 1.5mL/min, extraction time 2h.
4. CO as described in claim 12The method of means of supercritical extraction agar polyphenol, which is characterized in that fluid extracts in step 3
Pressure power is 20MPa.
5. CO as described in claim 12The method of means of supercritical extraction agar polyphenol, which is characterized in that temperature is extracted in step 3
It spends for 60 DEG C.
6. CO as described in claim 12The method of means of supercritical extraction agar polyphenol, which is characterized in that when being extracted in step 3
Between be 2h.
7. a kind of CO using as described in any in claim 1-62What the method for means of supercritical extraction agar polyphenol was extracted
The purposes of agar polyphenol, for inhibiting the activity of alpha-glucosidase and/or α-amylase.
8. a kind of CO using as described in any in claim 1-62What the method for means of supercritical extraction agar polyphenol was extracted
Application of the agar polyphenol in blood glucose is reduced.
9. a kind of CO using as described in any in claim 1-62What the method for means of supercritical extraction agar polyphenol was extracted
Agar polyphenol, is used to prepare antioxidant.
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| CN110051704A (en) * | 2019-06-05 | 2019-07-26 | 北部湾大学 | A kind of purposes of agar polyphenol extract as alpha-glucosidase restrainer |
| CN111418845A (en) * | 2020-05-25 | 2020-07-17 | 北部湾大学 | Preparation method of laver polyphenol extract and application of laver polyphenol extract |
| CN112980445A (en) * | 2021-03-26 | 2021-06-18 | 四川大学 | Method for extracting phenolic antioxidant from pepper oil processing by-product |
| CN115403634A (en) * | 2022-08-30 | 2022-11-29 | 集美大学 | Method for extracting polyphenol from agar industrial waste liquid by using ionic liquid and application thereof |
| CN117414690A (en) * | 2023-10-18 | 2024-01-19 | 四川冠山科技有限公司 | Sulfide remover and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110051704A (en) * | 2019-06-05 | 2019-07-26 | 北部湾大学 | A kind of purposes of agar polyphenol extract as alpha-glucosidase restrainer |
| CN111418845A (en) * | 2020-05-25 | 2020-07-17 | 北部湾大学 | Preparation method of laver polyphenol extract and application of laver polyphenol extract |
| CN112980445A (en) * | 2021-03-26 | 2021-06-18 | 四川大学 | Method for extracting phenolic antioxidant from pepper oil processing by-product |
| CN112980445B (en) * | 2021-03-26 | 2022-04-12 | 四川大学 | Method for extracting phenolic antioxidant from pepper oil processing by-product |
| CN115403634A (en) * | 2022-08-30 | 2022-11-29 | 集美大学 | Method for extracting polyphenol from agar industrial waste liquid by using ionic liquid and application thereof |
| CN117414690A (en) * | 2023-10-18 | 2024-01-19 | 四川冠山科技有限公司 | Sulfide remover and preparation method thereof |
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