CN108310197A - The preparation method of lily active material - Google Patents
The preparation method of lily active material Download PDFInfo
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- CN108310197A CN108310197A CN201810134392.9A CN201810134392A CN108310197A CN 108310197 A CN108310197 A CN 108310197A CN 201810134392 A CN201810134392 A CN 201810134392A CN 108310197 A CN108310197 A CN 108310197A
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- polyphenols
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- 241000234435 Lilium Species 0.000 title claims abstract description 101
- 239000011149 active material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000000284 extract Substances 0.000 claims abstract description 38
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 28
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 20
- 230000001954 sterilising effect Effects 0.000 claims description 19
- 238000004659 sterilization and disinfection Methods 0.000 claims description 19
- 239000006228 supernatant Substances 0.000 claims description 15
- 238000002137 ultrasound extraction Methods 0.000 claims description 11
- 238000001471 micro-filtration Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000006286 aqueous extract Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 6
- SLPPPCNWUHZRBG-UHFFFAOYSA-N S=CC(=O)O.CC1=CC=CC=C1 Chemical compound S=CC(=O)O.CC1=CC=CC=C1 SLPPPCNWUHZRBG-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000012467 final product Substances 0.000 claims description 2
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 2
- 230000000996 additive effect Effects 0.000 claims 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 26
- -1 DPPH free radical Chemical class 0.000 abstract description 8
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 230000008030 elimination Effects 0.000 abstract description 8
- 238000003379 elimination reaction Methods 0.000 abstract description 8
- 241000196324 Embryophyta Species 0.000 abstract description 6
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 5
- 235000013376 functional food Nutrition 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 5
- 231100000331 toxic Toxicity 0.000 abstract description 5
- 230000002588 toxic effect Effects 0.000 abstract description 5
- 229940088710 antibiotic agent Drugs 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 241000251468 Actinopterygii Species 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 7
- 241000220223 Fragaria Species 0.000 description 6
- 235000016623 Fragaria vesca Nutrition 0.000 description 6
- 235000011363 Fragaria x ananassa Nutrition 0.000 description 6
- 230000003385 bacteriostatic effect Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 241000607548 Aeromonas media Species 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 240000002234 Allium sativum Species 0.000 description 3
- 241000193830 Bacillus <bacterium> Species 0.000 description 3
- 244000063299 Bacillus subtilis Species 0.000 description 3
- 235000014469 Bacillus subtilis Nutrition 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000607142 Salmonella Species 0.000 description 3
- 241000863432 Shewanella putrefaciens Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 235000004611 garlic Nutrition 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- VYNUATGQEAAPAQ-UHFFFAOYSA-N 2-sulfonylacetic acid Chemical compound OC(=O)C=S(=O)=O VYNUATGQEAAPAQ-UHFFFAOYSA-N 0.000 description 1
- 240000007185 Albizia julibrissin Species 0.000 description 1
- 235000011468 Albizia julibrissin Nutrition 0.000 description 1
- 244000000383 Allium odorum Species 0.000 description 1
- 235000018645 Allium odorum Nutrition 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000723375 Colchicum Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 235000015979 Lilium brownii var viridulum Nutrition 0.000 description 1
- 244000039138 Lilium brownii var. viridulum Species 0.000 description 1
- 241001315001 Lilium concolor Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 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 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000401 methanolic extract Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 125000004646 sulfenyl group Chemical group S(*)* 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8967—Lilium, e.g. tiger lily or Easter lily
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/14—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
- A23B4/18—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/14—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
- A23B4/18—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
- A23B4/20—Organic compounds; Microorganisms; Enzymes
-
- 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
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/20—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing sulfur, e.g. dimethyl sulfoxide [DMSO], docusate, sodium lauryl sulfate or aminosulfonic acids
-
- 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
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
-
- 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
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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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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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
- A61K2236/30—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, 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses the preparation methods of lily active material, including：Water carries, alcohol extracting, extracts Polyphenols, compound.It has the beneficial effect that：Active material is extracted from lily floral leaf, bud, bulb, extracting method is simple and practicable, the full effect for also achieving lily utilizes, maximumlly its biological effectiveness is played, lily active material has preferable elimination effect to O2, OH and DPPH free radical, and it derives from natural plant component, and toxic side effect is relatively small, therefore in terms of the research of antibacterials and the exploitation of anti-oxidation functional food, there are preferable development and application potentiality.
Description
Technical field
The present invention relates to lily field of deep, more particularly, to the preparation method of lily active material.
Technical background
Lily, scientific name（Lilium brownii var. viridulum Baker）Also known as it strong another name for Sichuan Province, kind fragrant-flowered garlic, morningstar lily, falls
It is celestial, again step, Zhongting, sieve that rubs, loaded van, in meet flower, lily garlic, cook's garlic, garlic brain potato, silk tree etc., be Liliaceae lilium
（Scientific name：Lilium）Perennial herb bulbous plant, it is native to China, it is mainly distributed on the north such as east Asia, Europe, North America
Hemisphere Temperate Region in China, the whole world is it has been found that have at least 120 kinds, wherein 55 kinds originate in China.In recent years more have many by artificial
The new varieties of hybridization and generation, such as Lilium Pollyanna, Fragrant Lily, fiery lily.Bulb contains abundant starch, edible, also makees medicinal.
Lily removes to be contained containing protein 21.29%, fat 12.43%, reduced sugar 11.47%, starch 1.61% and calcium, phosphorus, iron, every hectogram
Outside the nutrients such as 1.443 milligrams of vitamin Bs, 21.2 milligrams of vitamin Cs, also containing some special nutritional ingredients, such as colchicum
A variety of alkaloids such as alkali.These ingredient comprehensive functions not only have the work(of good nutritious tonifying, but also to autumn in human body
A variety of Seasonal diseases have certain preventive and therapeutic effect caused by dry.Say that fresh lily bulb has mental-tranquilization, profit in Chinese medicine
It is the effect of lung cough-relieving, very useful to the people of eak after being ill.
Invention content
The purpose of the present invention is to provide the preparation methods of lily active material, and preparation method is simple for this, prepared
It is not added with noxious material in journey, and realizes the full effect utilization of lily floral leaf, bud, bulb, has maximumlly played lily
Biological effectiveness.
The present invention is directed to the problem of being mentioned in background technology, and the technical solution taken is：The preparation side of lily active material
Method, including：Water carries, alcohol extracting, extracts Polyphenols, compound, specifically includes following steps：
Water carries：Lily floral leaf, bud are weighed, crushed after being dried crosses 100-160 mesh sieve, 10-12 times of ultra-pure water is added, in 40-45
At a temperature of DEG C, using double ultrasonic extraction method 4-6 hours, supernatant is taken after centrifugation, with micro-filtration sterilization device filtration sterilization, vacuum refrigeration
Up to lily aqueous extract after drying；Lily floral leaf, bud water-soluble extractive to Shewanella putrefaciens, strawberry pseudomonad and
Aeromonas media have bacteriostatic activity, therefore can be applied to the flesh of fish it is fresh-keeping in；
Alcohol extracting：Water intaking carry after be suspended in sediment, the ethanol solution of 12-15 times of 90-98% is added, at a temperature of 40-45 DEG C,
Using double ultrasonic extraction method 1-1.5 hours, it is steamed into paste with Rotary Evaporators, micro-filtration sterilization device after ethyl alcohol is dissolved in and crosses and filter out
Bacterium, up to lily alcohol extract after vacuum freeze drying；Lily alcohol extract has suppression to strawberry pseudomonad and Aeromonas media
Bacterium activity can be developed into natural Novel antibacterial antistaling agent for the fresh-keeping industry of the flesh of fish, can effectively improve the fresh-keeping quality of the flesh of fish,
Extend flesh of fish shelf life；
Extract Polyphenols：Lily bulb is removed into mud, is cleaned, is dried in the shade naturally, 100-160 mesh sieve is smashed it through, takes lily bulb dry
Powder is in container, according to solid-liquid ratio 1g:30-45mL is added methanol solution and is carried using double supercritical ultrasonics technologies at a temperature of 30-35 DEG C
It takes 20-30 minutes, is centrifuged 10-12 minutes under the conditions of 0-4 DEG C, 12000-15000r/min later, collect supernatant, insoluble portion
Divide and repeat to extract, merge supernatant and the rotary evaporation Extraction solvent at 28-30 DEG C, is freeze-dried into powder to get more after concentration
Phenols extract；The methanolic extract of lily bulb is to bacillus subtilis, staphylococcus aureus, Bacillus cercus, sand
Door Salmonella, Escherichia coli, aerobacteria have certain inhibiting effect, while having preferably to O2-, OH and DPPH free radical
Elimination effect；
Compound：Lily aqueous extract, lily alcohol extract and Polyphenols extract are dissolved in the ethanol solution of 5-6 times of 50-70%,
Fully up to lily active material after dissolving；Active material is extracted from lily floral leaf, bud, bulb, extracting method is simple
Easy, the full effect for also achieving lily utilizes, and has maximumlly played its biological effectiveness, lily active material is to O2-, OH
There is preferable elimination effect with DPPH free radicals, and it derives from natural plant component, toxic side effect is relatively small, because
This has preferable development and application potentiality in terms of the research of antibacterials and the exploitation of anti-oxidation functional food.
Preferably, the supersonic frequency of bifrequency ultrasonic wave and sound intensity density are respectively 25-30kHz, 0.35-0.40W/
cm2With 45-50kHz, 0.45-0.60W/cm2；Bifrequency ultrasonic wave can not only accelerating medium particle movement and diffusion, while its
Cavitation can be overlapped mutually with vibration homogenization, and the effect that generated collapse effect disperses considerably beyond two ultrasonic waves adds
With, it can be effectively facilitated the diffusion and dissolution of active constituent in lily floral leaf, bud, bulb, reduce extraction time, raising extraction
Efficiency.
Preferably, extracting the hydrochloric acid solution containing 4.2-5.0% in the methanol solution in Polyphenols step, hydrochloric acid solution
Mass fraction be 10-15%, also containing 1.3-1.4's ‰（S）-（+）To toluene sulfenyl acetic acid；（S）-（+）To toluene Asia
Sulphonyl acetic acid is in the presence of the hydrochloric acid of very special quality multiple, the phenolic hydroxyl group that can be effectively promoted in lily bulb tissue
The dissolution and diffusion of substance so as to accelerate its extraction, and do not interfere with the property of phenolic hydroxyl group active material, hydrochloric acid with
（S）-（+）Toluene sulfenyl acetic acid can be eliminated during subsequent rotary evaporation, shadow will not be caused to the quality of product
It rings, that is, accelerates extraction efficiency, and improve the yield of aldehydes matter.
Compared with the prior art, the advantages of the present invention are as follows：1）（S）-（+）To toluene sulfenyl acetic acid in very special quality
In the presence of the hydrochloric acid of multiple, it can be effectively promoted the dissolution and diffusion of the phenolic hydroxyl group substance in lily bulb tissue,
So as to accelerate its extraction, the quality of product will not be impacted, that is, accelerate extraction efficiency, and improve aldehydes matter
Yield；2）Active material is extracted from lily floral leaf, bud, bulb, extracting method is simple and practicable, also achieves lily
Full effect utilizes, and has maximumlly played its biological effectiveness, lily active material to O2-, OH and DPPH free radical have compared with
Good elimination effect, and it derives from natural plant component, toxic side effect is relatively small, thus in the research of antibacterials and
In terms of the exploitation of anti-oxidation functional food, there are preferable development and application potentiality.
Specific implementation mode
The present invention program is described further below by embodiment：
Embodiment 1：
The preparation method of lily active material, includes the following steps：
1）Lily floral leaf, bud are weighed, crushed after being dried sieves with 100 mesh sieve, and 10 times of ultra-pure waters are added, and at a temperature of 40 DEG C, uses
Double ultrasonic extraction methods 4 hours, take supernatant after centrifugation, with micro-filtration sterilization device filtration sterilization, up to lily after vacuum freeze drying
Water extract；2）Water intaking carry after be suspended in sediment, 12 times 90% of ethanol solution is added, at a temperature of 40 DEG C, using double ultrasounds
Wave method is extracted 1 hour, is steamed into paste with Rotary Evaporators, is dissolved in micro-filtration sterilization device filtration sterilization after ethyl alcohol, vacuum freeze drying
Afterwards up to lily alcohol extract；3）Lily bulb is removed into mud, is cleaned, is dried in the shade naturally, 100 mesh sieve is smashed it through, takes lily bulb dry
Powder is in container, according to solid-liquid ratio 1g:30mL is added methanol solution and is divided using double ultrasonic extraction methods 20 at a temperature of 30 DEG C
Clock centrifuges 10 minutes under the conditions of 0 DEG C, 12000r/min later, collects supernatant, and insoluble part repeats to extract, and merges supernatant
Liquid and the rotary evaporation Extraction solvent at 28 DEG C are freeze-dried into powder after concentration to get Polyphenols extract；4）Lily water is carried
Object, lily alcohol extract and Polyphenols extract are dissolved in 5 times 50% of ethanol solution, fully up to lily active matter after dissolving
Matter.
Embodiment 2：
The preparation method of lily active material, includes the following steps：
1）Water carries：Lily floral leaf, bud are weighed, crushed after being dried crosses 140 mesh sieve, 10 times of ultra-pure waters is added, in 42 DEG C of temperature
Under, using double ultrasonic extraction methods 5 hours, supernatant is taken after centrifugation, with micro-filtration sterilization device filtration sterilization, after vacuum freeze drying i.e.
Obtain lily aqueous extract；Lily floral leaf, bud water-soluble extractive to Shewanella putrefaciens, strawberry pseudomonad and intermediate gas list
Born of the same parents bacterium have bacteriostatic activity, therefore can be applied to the flesh of fish it is fresh-keeping in；
2）Alcohol extracting：Water intaking carry after be suspended in sediment, 14 times 95% of ethanol solution is added, at a temperature of 42 DEG C, using double super
Sonic method extracts 1.5 hours, is steamed into paste with Rotary Evaporators, is dissolved in micro-filtration sterilization device filtration sterilization after ethyl alcohol, vacuum refrigeration
Up to lily alcohol extract after drying；Lily alcohol extract has bacteriostatic activity to strawberry pseudomonad and Aeromonas media, can incite somebody to action
It is developed is used for the fresh-keeping industry of the flesh of fish at natural Novel antibacterial antistaling agent, can effectively improve the fresh-keeping quality of the flesh of fish, extend flesh of fish goods
The frame phase；
3）Extract Polyphenols：Lily bulb is removed into mud, is cleaned, is dried in the shade naturally, 120 mesh sieve is smashed it through, takes lily bulb dry powder
In container, according to solid-liquid ratio 1g:35mL is added methanol solution and is divided using double ultrasonic extraction methods 20 at a temperature of 30-35 DEG C
Clock centrifuges 10 minutes under the conditions of 1 DEG C, 14000r/min later, collects supernatant, and insoluble part repeats to extract, and merges supernatant
Liquid and the rotary evaporation Extraction solvent at 28 DEG C are freeze-dried into powder after concentration to get Polyphenols extract；The first of lily bulb
Alcohol extracting thing is to bacillus subtilis, staphylococcus aureus, Bacillus cercus, salmonella, Escherichia coli, aerobacteria
There is certain inhibiting effect, while having preferable elimination effect to O2-, OH and DPPH free radical；
Compound：Lily aqueous extract, lily alcohol extract and Polyphenols extract are dissolved in 6 times 60% of ethanol solution, it is fully molten
Up to lily active material after solution；Active material is extracted from lily floral leaf, bud, bulb, extracting method is simple and practicable, also
The full effect for realizing lily utilizes, and has maximumlly played its biological effectiveness, lily active material is to O2-, OH and DPPH
Free radical has preferable elimination effect, and it derives from natural plant component, and toxic side effect is relatively small, therefore in antibacterial
In terms of the research of drug and the exploitation of anti-oxidation functional food, there are preferable development and application potentiality.
Embodiment 3：
The preparation method of lily active material, including：Water carries, alcohol extracting, extracts Polyphenols, compound, specifically includes following steps：
Water carries：Lily floral leaf, bud are weighed, crushed after being dried crosses 160 mesh sieve, 12 times of ultra-pure waters is added, at a temperature of 45 DEG C,
Using double ultrasonic extraction methods 6 hours, supernatant is taken after centrifugation, with micro-filtration sterilization device filtration sterilization, after vacuum freeze drying to obtain the final product
Lily aqueous extract；Lily floral leaf, bud water-soluble extractive to Shewanella putrefaciens, strawberry pseudomonad and intermediate gas unit cell
Bacterium have bacteriostatic activity, therefore can be applied to the flesh of fish it is fresh-keeping in；
Alcohol extracting：Water intaking carry after be suspended in sediment, 15 times 98% of ethanol solution is added, at a temperature of 45 DEG C, using double ultrasounds
Wave method is extracted 1.5 hours, and paste is steamed into Rotary Evaporators, is dissolved in micro-filtration sterilization device filtration sterilization after ethyl alcohol, and vacuum refrigeration is dry
Up to lily alcohol extract after dry；Lily alcohol extract has bacteriostatic activity to strawberry pseudomonad and Aeromonas media, can be by it
Natural Novel antibacterial antistaling agent is developed into for the fresh-keeping industry of the flesh of fish, the fresh-keeping quality of the flesh of fish can be effectively improved, extend flesh of fish shelf
Phase；
Extract Polyphenols：By lily bulb go mud, clean, dry in the shade naturally, smash it through 160 mesh sieve, take lily bulb dry powder in
In container, according to solid-liquid ratio 1g:Methanol solution is added in 45mL, at a temperature of 35 DEG C, using double ultrasonic extraction methods 30 minutes, it
Centrifuged 12 minutes under the conditions of 4 DEG C, 15000r/min afterwards, collect supernatant, insoluble part repeats to extract, merge supernatant and in
Rotary evaporation Extraction solvent at 30 DEG C is freeze-dried into powder after concentration to get Polyphenols extract；The methanol of lily bulb extracts
Object has centainly bacillus subtilis, staphylococcus aureus, Bacillus cercus, salmonella, Escherichia coli, aerobacteria
Inhibiting effect, while having preferable elimination effect to O2-, OH and DPPH free radical；
Compound：Lily aqueous extract, lily alcohol extract and Polyphenols extract are dissolved in 6 times 70% of ethanol solution, it is fully molten
Up to lily active material after solution；Active material is extracted from lily floral leaf, bud, bulb, extracting method is simple and practicable, also
The full effect for realizing lily utilizes, and has maximumlly played its biological effectiveness, lily active material is to O2-, OH and DPPH
Free radical has preferable elimination effect, and it derives from natural plant component, and toxic side effect is relatively small, therefore in antibacterial
In terms of the research of drug and the exploitation of anti-oxidation functional food, there are preferable development and application potentiality.
The supersonic frequency of bifrequency ultrasonic wave and sound intensity density are respectively 28kHz, 0.35W/cm2With 46kHz, 0.45W/
cm2；Bifrequency ultrasonic wave can not only accelerating medium particle movement and diffusion, while its cavitation with vibration homogenization can phase
Mutually superposition, generated collapse effect considerably beyond the effect adduction of two ultrasonic waves dispersions, can be effectively facilitated lily floral leaf,
The diffusion and dissolution of active constituent in bud, bulb reduce extraction time, improve extraction efficiency.
It is containing 4.5% hydrochloric acid solution, the mass fraction of hydrochloric acid solution in methanol solution in extraction Polyphenols step
12%, also containing 1.3 ‰（S）-（+）To toluene sulfenyl acetic acid；（S）-（+）To toluene sulfenyl acetic acid in very special quality
In the presence of the hydrochloric acid of multiple, it can be effectively promoted the dissolution and diffusion of the phenolic hydroxyl group substance in lily bulb tissue,
So as to accelerate its extraction, and do not interfere with the property of phenolic hydroxyl group active material, hydrochloric acid with（S）-（+）To toluene Asia sulphur
Ethyl acetoacetic acid can be eliminated during subsequent rotary evaporation, will not be impacted to the quality of product, that is, accelerate extraction effect
Rate, and improve the yield of aldehydes matter.
Routine operation in operating procedure of the present invention is well known to those skilled in the art, herein without repeating.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. the preparation method of lily active material, it is characterised in that：The preparation method of the lily active material includes：
Water carries：By lily floral leaf, bud crushed after being dried, 100-160 mesh sieve is crossed, 10-12 times of ultra-pure water is added, extracts and centrifuges
Take supernatant, micro-filtration sterilization device filtration sterilization, up to lily aqueous extract after vacuum freeze drying；
Alcohol extracting：Ethanol solution is added in the suspended matter and sediment fetched water after carrying, and using double ultrasonic extraction method 1-1.5 hours, uses
Rotary Evaporators are steamed into paste, are dissolved in micro-filtration sterilization device filtration sterilization after ethyl alcohol, up to lily alcohol extract after vacuum freeze drying；
Extract Polyphenols：Lily bulb is removed into mud, is cleaned, is dried in the shade naturally, 100-160 mesh sieve is smashed it through, takes lily bulb dry
Powder is added methanol solution and, using double ultrasonic extraction method 20-30 minutes, is received after centrifugation at a temperature of 30-35 DEG C in container
Collect supernatant, insoluble part repeats to extract, merges supernatant and the rotary evaporation Extraction solvent at 28-30 DEG C, freezed after concentration
Powder is dried to get Polyphenols extract；
Compound：Lily aqueous extract, lily alcohol extract and Polyphenols extract are dissolved in ethanol solution, fully after dissolving to obtain the final product
Lily active material.
2. the preparation method of lily active material according to claim 1, it is characterised in that：In the aqueous extraction step, carry
It was 40-45 DEG C to take temperature, using double ultrasonic extraction method 4-6 hours.
3. the preparation method of lily active material according to claim 1 or 2, it is characterised in that：The water carries, alcohol extracting with
It extracts in Polyphenols step, supersonic frequency and the sound intensity density of bifrequency ultrasonic wave are respectively 25-30kHz, 0.35-0.40W/
cm2With 45-50kHz, 0.45-0.60W/cm2。
4. the preparation method of lily active material according to claim 1, it is characterised in that：In the alcohol extracting step, institute
The mass fraction of the ethanol solution of addition is 90-98%, and additive amount is 12-15 times of suspended matter and sediment, and Extracting temperature is
40-45℃。
5. the preparation method of lily active material according to claim 1, it is characterised in that：The extraction Polyphenols step
In, solid-liquid ratio when methanol solution is added is 1g:30-45mL.
6. the preparation method of lily active material according to claim 1, it is characterised in that：The extraction Polyphenols step
In, after methanol solution is added and extracts, centrifuged 10-12 minutes under the conditions of 0-4 DEG C, 12000-15000r/min.
7. the preparation method of lily active material according to claim 1, it is characterised in that：In the compound step, second
The mass fraction of alcoholic solution is 50-70%, additive amount be lily aqueous extract, lily alcohol extract and Polyphenols extract quality and
5-6 times.
8. the preparation method of lily active material according to claim 1, it is characterised in that：The extraction Polyphenols step
In, the mass fraction of the hydrochloric acid solution containing 4.2-5.0% in methanol solution, hydrochloric acid solution is 10-15%, also contains 1.3-
1.4 ‰（S）-（+）To toluene sulfenyl acetic acid.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116211955A (en) * | 2023-01-13 | 2023-06-06 | 南京农业大学 | Lily bulb antioxidant extraction method |
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