CN108743632A - A kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba - Google Patents

A kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba Download PDF

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Publication number
CN108743632A
CN108743632A CN201810389939.XA CN201810389939A CN108743632A CN 108743632 A CN108743632 A CN 108743632A CN 201810389939 A CN201810389939 A CN 201810389939A CN 108743632 A CN108743632 A CN 108743632A
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ginkgo
powder
gingko
fruits
removal
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CN108743632B (en
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杨胜利
杨锡
邵泽辉
潘芸
程坷伟
陶缘
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Zhejiang University of Technology ZJUT
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/16Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Abstract

A kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba, the method are:Fresh gingko is taken, after decapsidate, kind skin, through crushing, drying, is ground up, sieved, obtains ginkgo powder;Gained ginkgo powder is mixed with water, neutral proteinase is then added, 1~1.5h is digested under conditions of 38~45 DEG C of temperature, 20~40kHz of ultrasonic frequency, is filtered later, collects filter cake;Filter cake is mixed with ethanol water, gained mixed liquor is rotated under conditions of 45~60 DEG C of temperature, 20~40kHz of ultrasonic frequency, 30~70Pa of pressure to the 1/5~1/4 of initial volume, gained concentrate is filtered, solid is filtered out and is dried to obtain gingko powder, complete the removal of ginkgoic acid;Minimizing technology product recovery rate of the present invention is high, ginkgoic acid removal effect is good, and ginkgo acid content is less than 3 μ g/g;Present invention process is simple, and agents useful for same is easy to get, is safe, and production cost is low, it is easy to accomplish industrialization.

Description

A kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba
(1) technical field
The present invention relates to the methods that a kind of ultrasonic wave auxiliary removes ginkgoic acid from gingko.
(2) background technology
Gingko (scientific name:Ginkgo biloba) also known as duck bottom sediment, mental eye, Buddhist refer to mandarin orange, ginkgo, Gong Sunshuzi are ginkgoes Benevolence.Often edible gingko can be expanded capilary, promoted blood circulation, make one skin, face with enriching yin face nourishing antidebilitation It is ruddy, it is in high spirits, promote longevity, is the special delicacies of suitable to people of all ages health food and the upper visitor that entertains the state guests.In benevolence Glycosides displayed, bitter lactones are to diseases such as cerebral thrombus, senile dementia, hypertension, hyperlipidemia, coronary heart disease, artery sclerosis, Agings Disease also has special prevention and treatment effect.
Gingko is broadly divided into two kinds of medicinal gingko and edible gingko, and medicinal gingko slightly astringent taste eats gingko clean taste. Gingko kernel in addition to containing starch, protein, fat, carbohydrate, also contain vitamin C, riboflavin, carrotene, calcium, phosphorus, The trace element such as iron, potassium, magnesium and ginkgoic acid, bilobol, five carbon polysaccharide, the ingredients such as fat sterol are full of nutrition.Mild-natured, sweet in flavor, Slightly bitter is puckery, toxic.The world of medicine thinks at present, and children eat it raw 7~15 pieces, you can causes to be poisoned, frying rear toxicity reduces, but primary The amount of eating can not be excessive.
There are many gingko product currently on the market, but there are no the removal specifically for toxic components such as Ginkgolic Acids in Fruits of Ginkgo biloba Method.
(3) invention content
The present invention provides a kind of method that ultrasonic wave assists removal Ginkgolic Acids in Fruits of Ginkgo biloba, the method for the present invention combines ultrasound The strong point of wave method and protease hydrolyzed method, has abandoned the high-quality of single method and the shortcomings that low cost is difficult to merge, this method The effect that nutritional ingredient is destroyed less, ginkgoic acid removal rate is high in gingko can be kept, and ginkgo protein is hydrolyzed to small peptide and ammonia Base acid, more conducively absorption of human body utilize, and can reduce energy consumption reduction processing cost.
Technical solution of the present invention it is as follows:
A kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba, the method are:
(1) fresh gingko (commercially available) is taken, after decapsidate, kind skin, through crushing, drying, is ground up, sieved, obtains ginkgo powder;
Specifically, step (1) crushing, operating method that is dry, being ground up, sieved are:Shell will be eliminated, plant skin Fresh gingko, which is put into pulverizer, is ground into paste, and it is 8~10% then to be dried in 60~80 DEG C to moisture, then through grinding Mill crosses 150~180 mesh sieve, obtains ginkgo powder;
(2) ginkgo powder obtained by step (1) is pressed into solid-liquid ratio 1 with water:20~30 (g:ML it) mixes, neutral protein is then added Enzyme digests 1~1.5h under conditions of 38~45 DEG C of temperature, 20~40kHz of ultrasonic frequency, filters later, collects filter cake (nothing Need drying);
The mass ratio of the neutral proteinase and ginkgo powder is 1:50~100;
The enzyme activity of the neutral proteinase is 50000U/g;
(3) filter cake obtained by step (2) is taken, by solid-liquid ratio 1:40~50 (g:ML) with the ethanol water of volume fraction 95~98% Solution mix, obtain mixed liquor, by gained mixed liquor in 45~60 DEG C of temperature, 20~40kHz of ultrasonic frequency, pressure 30~ Revolving obtains concentrate, gained concentrate is filtered, solid is filtered out to the 1/5~1/4 of initial volume under conditions of 70Pa It is dried to obtain gingko powder, completes the removal of ginkgoic acid;
It is described filter out solid in 60~80 DEG C it is dry to moisture be 8~10%, obtain gingko powder;
Gained gingko powder can detect ginkgo acid content by HPLC at 310nm.
Compared with prior art, the invention has the advantages that and advantageous effect:
(1) minimizing technology product recovery rate of the present invention is high, ginkgoic acid removal effect is good, and ginkgo acid content is less than 3 μ g/g;
(2) present invention process is simple, and agents useful for same is easy to get, is safe, and production cost is low, it is easy to accomplish industrialization.
(4) specific implementation mode
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in This:
The fresh gingko used in embodiment is that Taixing giant Buddha refers to gingko;Neutral proteinase is purchased from Novi's letter (China) biology Technology Co., Ltd., enzyme activity 50000U/g.
Embodiment 1
(1) commercially available fresh gingko is taken, except decapsidate, kind skin, is then placed in pulverizer and is ground into paste, paste is set It at 80 DEG C dry (being 10% to moisture) for 24 hours, then is ground, crosses 150 mesh sieve, obtain ginkgo powder.
(2) electronic analytical balance weighs 10.00g ginkgo powders, is mixed with 200mL water, and 0.1g neutral proteinases are then added, 20kHz ultrasonic waves auxiliary is heated to 38 DEG C of enzymolysis 1h under promoting, filter cake is collected in filtering.
(3) filter cake obtained by step (2) is taken, is mixed with the ethanol water of 400mL volume fractions 95%, in 50 DEG C of thermostatted waters In bath, under 20kHz ultrasonic waves auxiliary promotes, 3h is rotated in 30Pa, the volume of gained concentrate is the 1/5 of initial volume, it After filter, filter cake dry (being 10% to moisture) for 24 hours at 80 DEG C obtains gingko powder 9.32g.
Gingko powder prepared by the present embodiment is white, and it is 2.84 μ g/g that HPLC, which detects ginkgoic acid mass content,.
Embodiment 2
(1) commercially available fresh gingko is taken, except decapsidate, kind skin, is then placed in pulverizer and is ground into paste, paste is set It at 80 DEG C dry (being 10% to moisture) for 24 hours, then is ground, crosses 180 mesh sieve, obtain ginkgo powder.
(2) electronic analytical balance weighs 10.00g ginkgo powders, is mixed with 250mL water, and 0.15g neutral proteins are then added Enzyme, 30kHz ultrasonic waves auxiliary are heated to 40 DEG C of enzymolysis 1.5h under promoting, filter cake is collected in filtering.
(3) filter cake obtained by step (2) is taken, is mixed with the ethanol water of 500mL volume fractions 95%, in 50 DEG C of thermostatted waters In bath, under 30kHz ultrasonic waves auxiliary promotes, 3.5h is rotated in 50Pa, the volume of gained concentrate is the 1/4 of initial volume, It filters later, filter cake dry (being 10% to moisture) for 24 hours at 80 DEG C obtains gingko powder 9.27g.
Gingko powder prepared by the present embodiment is white, and it is 2.61 μ g/g that HPLC, which detects ginkgoic acid mass content,.
Embodiment 3
(1) commercially available fresh gingko is taken, except decapsidate, kind skin, is then placed in pulverizer and is ground into paste, paste is set It at 80 DEG C dry (being 10% to moisture) for 24 hours, then is ground, crosses 180 mesh sieve, obtain ginkgo powder.
(2) electronic analytical balance weighs 10.00g ginkgo powders, is mixed with 300mL water, and 0.2g neutral proteinases are then added, 40kHz ultrasonic waves auxiliary is heated to 45 DEG C of enzymolysis 1.5h under promoting, filter cake is collected in filtering.
(3) filter cake obtained by step (2) is taken, is mixed with the ethanol water of 400mL volume fractions 98%, in 60 DEG C of thermostatted waters In bath, under 40kHz ultrasonic waves auxiliary promotes, 3h is rotated in 60Pa, the volume of gained concentrate is the 1/5 of initial volume, it After filter, filter cake dry (being 10% to moisture) for 24 hours at 80 DEG C obtains gingko powder 9.35g.
Gingko powder prepared by the present embodiment is white, and it is 2.96 μ g/g that HPLC, which detects ginkgoic acid mass content,.
Comparative example
Currently without the technique for carrying out de- ginkgoic acid to gingko, all it is simple boiling, has and removed from ginkgo biloba p.e Ginkgoic acid.Such as a kind of method in removal ginkgo biloba extract described in the method (CN201510147957.3) of ginkgoic acid.It should Method needs special foam separator, uses a large amount of chemical reagent NaHCO3, Span-40 and Tween-20, ginkgoic acid after removal Content is 4.3ppm.Specially:
(1) raw material weighing:Weigh commercially available 25g ginkgo biloba extracts.
(2) formulated suspension:It is added in the beaker for filling commercially available ginkgo biloba extract, is sufficiently stirred with 700mL water, made Extract dissolves as far as possible.
(3) saturation NaHCO is added3Solution adjusts pH, makes to be equal to 8.
(4) dosage of surfactant:Surfactant is weighed, the surfactant is mixed for Span-40 and Tween-20 Object is closed, the mass ratio of the two is 1:2.
(5) surfactant will be added in above-mentioned suspension, be transferred in foam separator after mixing.
(6) after the completion of above-mentioned work, air is passed through from foam separator bottom at room temperature.The gas velocity of control air exists 80mL/min or so.
(7) foam taken out of foam separator upper end is collected, foam is the solution of composition containing ginkgo acid.Place in foam separator Solution after reason is the solution for removing ginkgoic acid, and with high performance liquid chromatography, chromatographic column is HiQ sil C18 columns, mobile phase For methanol 3%HAc solution, flow velocity 1mL/min, Detection wavelength 310nm, 40 DEG C of column temperature.By the solution of above-mentioned removal ginkgoic acid Concentration, dry to get to removal ginkgoic acid ginkgo biloba extract 22.74g.This method converts to obtain extract product to the end after measuring Middle ginkgo acid content is 4.3ppm.
The ethyl alcohol of the method for the present invention use environment close friend is assisted as solvent using physical method ultrasonic wave, and product silver Apricot acid content is far below above-mentioned technology, has a clear superiority.

Claims (4)

1. a kind of method of ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba, which is characterized in that the method is:
(1) fresh gingko is taken, after decapsidate, kind skin, through crushing, drying, is ground up, sieved, obtains ginkgo powder;
(2) ginkgo powder obtained by step (1) is pressed into solid-liquid ratio 1 with water:20~30 mixing, are then added neutral proteinase, in temperature 38~45 DEG C, 1~1.5h is digested under conditions of 20~40kHz of ultrasonic frequency, filter later, collect filter cake;
(3) filter cake obtained by step (2) is taken, by solid-liquid ratio 1:40~50 mix with the ethanol water of volume fraction 95~98%, Mixed liquor is obtained, by gained mixed liquor in 45~60 DEG C of temperature, the condition of 20~40kHz of ultrasonic frequency, 30~70Pa of pressure It is lower revolving to the 1/5~1/4 of initial volume, obtain concentrate, gained concentrate be filtered, filter out solid be dried to obtain it is white Fruit powder completes the removal of ginkgoic acid.
2. the method for ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba as described in claim 1, which is characterized in that step (1) is described It crushes, is dry, operating method that is being ground up, sieved is:The fresh gingko for eliminating shell, kind skin is put into pulverizer and is ground into Paste, it is 8~10% then to be dried in 60~80 DEG C to moisture, then ground, crosses 150~180 mesh sieve, obtains ginkgo Powder.
3. the method for ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba as described in claim 1, which is characterized in that in step (2), institute The mass ratio for stating neutral proteinase and ginkgo powder is 1:50~100;The enzyme activity of the neutral proteinase is 50000U/g.
4. the method for ultrasonic wave auxiliary removal Ginkgolic Acids in Fruits of Ginkgo biloba as described in claim 1, which is characterized in that in step (3), institute It is 8~10% to state and filter out solid in 60~80 DEG C of dryings to moisture, obtains gingko powder.
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Publication number Priority date Publication date Assignee Title
CN110463910A (en) * 2019-08-29 2019-11-19 湖北金银丰食品有限公司 A kind of functional form nutrition fine dried noodles being eaten for a long time and production method

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