CN106880699A - The method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro- - Google Patents

The method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro- Download PDF

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Publication number
CN106880699A
CN106880699A CN201710139512.XA CN201710139512A CN106880699A CN 106880699 A CN106880699 A CN 106880699A CN 201710139512 A CN201710139512 A CN 201710139512A CN 106880699 A CN106880699 A CN 106880699A
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micro
catechin
golden
cut
tea
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徐永平
赛璇
贺栋业
李晓宇
王丽丽
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Dalian University of Technology
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Dalian University of Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/82Theaceae (Tea family), e.g. camellia
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY 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
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY 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
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY 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 TOILETRY 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

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Pyrane Compounds (AREA)
  • Tea And Coffee (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of using micro- method cut and help interaction technology to improve Camellia nitidissima extract catechin dissolution rate, including golden flower tea fresh leaves are cleaned, de-enzyme, dry, after crushing, after adding physics auxiliary agent superfine grinding, ultrasonic water is extracted, and is taken extract solution vacuum freeze drying and is obtained final product golden camellia tea water extract.The inventive method helps interaction technology assisted extraction golden camellia tea catechin using micro- cutting, it is micro- cut help powdery state under can effectively improve catechin dissolubility in aqueous, and golden camellia tea powder is crushed evenly, grain diameter is smaller, distribution of particles evenly, can further improve the eduction rate of catechin.The present invention is extracted using ultrasonic wave added water, not only greatly reduces active component dissolution time, is avoided that organic solvent is used again, and process is simple is cost-effective, is more beneficial for industrialization.

Description

The method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro-
Technical field
It is more particularly to a kind of to help interaction technology to improve using micro- cutting the present invention relates to active components of plants extractive technique field The method of Camellia nitidissima extract catechin dissolution rate.
Background technology
Camellia nitidissima [Camellia nitidissima Chi] category Theaceae (Theaceae) Camellia (Camellia) gold Flower Thea section (Camellia Section Chrysantha Chang), is uniquely have golden yellow dyeing defect in camellia family The kind of valve, is described as " tea race queen ", " plant kingdom giant panda " etc., has been listed in country-level, the rare protection in two grades of the world Plant, and new resource food is classified as by No. 9 bulletin of the Ministry of Public Health of China in 2010.Golden flower camellias and leaf are Zhuang nationality in Guangxi biography among the people System medication, with medical value higher,《Guangxi Chinese medicine standard》Record, the nature and flavor of Camellia nitidissima are slight bitter, puckery, are put down, function It is clearing heat and detoxicating, inducing diuresis to remove edema with curing mainly, for sphagitis, dysentery, ephritis, hypertension, irregular menstruation etc..Contain in golden camellia tea There are various effective medicinal ingredients, pharmaceutical research proves there is anti-inflammation, and anti-oxidant, antitumor, reducing blood lipid is hypoglycemic, resists The functions such as allergy, antianxiety depression, wherein golden flower tea catechins are a kind of more active skull cap components of research, and it is in medicine side The application in face has preferable application prospect, therefore the extraction of active component is separated into a technical barrier.
In the last few years, many domestic and foreign scholars constantly to plant effective active composition extract technique groped with it is excellent Change, some new extractions and isolation technics constantly emerge in large numbers appearance, such as microwave, ultrasonic wave, overcritical, although these new technologies There is significant progress than conventional art, but the low problem of active ingredient poorly water-soluble, availability is not solved fundamentally also Certainly, and some technologies due to equipment it is special, be also only limitted to laboratory research, and may not apply to Industrialized Production Practice.Can See, the imperfection of extractive technique is always to govern plant effective active composition deeper into research and the key of development and application Problem.Therefore, the extraction efficiency of active ingredient is improved, reduces cost develops skill maturity so as to reach industrialized production The exploitation of new technology is extremely urgent.Patent of invention:One kind is used for effective plant component extracting process, granted patent number: ZL200510130852.3, its main technical scheme is that the plant material that will be extracted is crushed, to adding 0.5 in plant meal The chemical assistant of~20% solid base, solid acid, sucrose or salt compounds powder, and fragility or sharp property inert material one Rise processed, from water or ethanol dissolution process product, separate and collect soluble constituents obtain active ingredient, vegetable active into Point extraction efficiency is low, and elapsed time is long.Therefore, these problems demands are solved.
The content of the invention
A kind of micro- cutting it is an object of the invention to provide utilization ultrasonic wave added helps interaction technology to extract golden flower tea catechins Method, improve golden flower tea catechin dissolutions amount and speed.
To reach above-mentioned purpose, interaction technology is helped to improve Camellia nitidissima extract catechin with micro- cutting the invention provides one kind The method of dissolution rate, comprises the following steps:
S1, golden flower tea fresh leaves are taken, cleaned, de-enzyme dry, pulverize under vacuum condition, cross 60~200 mesh sieves, obtain Camellia nitidissima Ye Fen;
S2, the physics auxiliary agent that its quality 1%~4% is accounted for addition in golden camellia tea powder obtained in step S1, grinding 10min, obtains micro- cutting and helps powder;The physics auxiliary agent is sharp property material;
S3, micro- cutting obtained in step S2 is helped into powder and water by solid-liquid ratio 1g:15mL is sufficiently mixed, ultrasound 30min at 70 DEG C, Filtering extract solution, collects to obtain filtrate;The supersonic frequency is 40KHz, power is 100W;
S4, by the filtrate freeze-drying obtained by step S3, obtain golden camellia tea water extract dry powder.
Step S4 is by the filtrate freeze-drying obtained by step S3 and recycle-water.
Under preferred embodiment, the de-enzyme described in step S1 is microwave high-temperature de-enzyme.
Under preferred embodiment, sharp property material described in step S2 is oyster shell whiting.
Technological innovation of the invention is:
1st, the present invention extracts new technology as golden flower tea catechins, can effectively extract golden flower tea extractions and catechin contains Amount, 20g raw material can obtain extract 3.65g~3.95g, and 1.93 times, catechin content are improved compared with traditional extraction process 2.49mg/g~2.66mg/g is reached, 4.59 times are improved compared with traditional extraction process.
2nd, the present invention utilizes ultrasound assisted extraction, and 30min is shorten to by original immersion 24h, greatly reduces catechin molten Go out the time, save the operating time, improve extraction efficiency.
3rd, the present invention cuts the mutual technology that helps using micro-, and animal-plant material cluster of grains is by micro- shear clasmatosis, cell surface Fresh tangent plane is produced, group or intermolecular mutual absorption or effect occur between auxiliary agent and active ingredient, change active ingredient Micro-property, surface can increase, and specific surface area increase, adsorptivity and polarity increase, by it is micro- cut help interaction technical finesse after The micro- dissolubility for helping powder in water of cutting for obtaining is greatly improved.Present invention comprehensive utilization ultrasonic technique helps interaction technology with micro- cutting Effectively combine and improve golden flower tea extractions recovery rate and catechin content, reduce the consumption of organic solvent, improve the ring for existing Border pollution problem;It is cost-effective and present invention process makees simple, it is more beneficial for industrialization.
Brief description of the drawings
Fig. 1 is the golden camellia tea particle size distribution figure of different pulverization process.
Fig. 2 is 60 mesh sieve golden camellia tea particulate scan electron microscopes.
Fig. 3 is 200 mesh sieve golden camellia tea particulate scan electron microscopes.
Fig. 4 is that micro- cutting processes golden camellia tea particulate scan electron microscope.
Fig. 5 is that micro- cutting helps treatment golden camellia tea particulate scan electron microscope.
Fig. 6 is different pulverization process golden camellia tea extract recovery rate figures.
Fig. 7 is catechin canonical plotting.
Fig. 8 is catechin content figure in different pulverization process golden camellia tea extracts.
Specific embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with Any mode limits the present invention.
Specific embodiment of the invention is described in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
Using micro- method cut and help interaction technology to improve Camellia nitidissima extract catechin dissolution rate, with golden camellia tea as former Material, comprises the following steps:
(1) golden flower tea fresh leaves are taken, is cleaned, microwave high-temperature de-enzyme, vacuum condition is dried, then by dried golden camellia tea Crush, cross 60 mesh sieves, obtain golden camellia tea powder, golden camellia tea grain diameter is shown in Fig. 1, golden camellia tea particulate scan electron microscope such as Fig. 2;
(2) the mesh powder 20g of golden camellia tea 60 is taken, by solid-liquid ratio 1g:15mL adds 300mL water to be sufficiently mixed, and is in frequency 40KHz, power are ultrasonic extraction 30min under 100W, the ul-trasonic irradiation that temperature is 70 DEG C, filter extract solution, collect to obtain filtrate;
(4) filtrate is carried out into freeze-drying by vacuum freeze drier, reclaims extractant-water, obtain golden camellia tea water Extract dry powder, obtains dry powder 2.26g, 2.02g, 1.96g, recovery rate analysis such as Fig. 6;
(5) by golden camellia tea dry composition into certain density solution to be measured, with catechin as standard items, standard curve is such as Fig. 7, detects that catechin content is 0.057mg/ to catechin content in extract using vanillic aldehyde-concentrated hydrochloric acid development process G, 0.058mg/g, 0.048mg/g, extract result statistics such as Fig. 8.
Embodiment 2
Using micro- method cut and help interaction technology to improve Camellia nitidissima extract catechin dissolution rate, with golden camellia tea as former Material, comprises the following steps:
(1) golden flower tea fresh leaves are taken, is cleaned, microwave high-temperature de-enzyme, vacuum condition is dried, then by dried golden camellia tea Crush, cross 200 mesh sieves, obtain golden camellia tea powder, golden camellia tea grain diameter is shown in Fig. 1, and golden camellia tea particulate scan electron microscope is as schemed 3;
(2) the mesh powder 20g of golden camellia tea 200 is taken, by solid-liquid ratio 1g:15mL adds 300mL water to be sufficiently mixed, and is in frequency 40KHz, power are ultrasonic extraction 30min under 100W, the ul-trasonic irradiation that temperature is 70 DEG C, filter extract solution, collect to obtain filtrate;
(4) filtrate is carried out into freeze-drying by vacuum freeze drier, reclaims extractant-water, obtain golden camellia tea water Extract dry powder, obtains dry powder 2.34g, 2.36g, 2.48g, recovery rate analysis such as Fig. 6;
(5) by golden camellia tea dry composition into certain density solution to be measured, with catechin as standard items, standard curve is such as Fig. 7, is detected using vanillic aldehyde-concentrated hydrochloric acid development process to catechin content in extract, catechin content be 1.99mg/g, 2.19mg/g, 2.18mg/g, extract result statistics such as Fig. 8.
Embodiment 3
Using micro- method cut and help interaction technology to improve Camellia nitidissima extract catechin dissolution rate, with golden camellia tea as former Material, comprises the following steps:
(1) golden flower tea fresh leaves are taken, is cleaned, microwave high-temperature de-enzyme, vacuum condition is dried, then by dried golden camellia tea Crush, cross 60 mesh sieves, obtain golden camellia tea powder;
(2) the mesh powder 500g of golden camellia tea powder 60 is taken, is put into vibromill and is ground 10min, obtained and micro- cut powder, golden camellia tea Grain diameter is shown in Fig. 1, golden camellia tea particulate scan electron microscope such as Fig. 4;
(3) take that golden camellia tea is micro- to cut powder 20g, by solid-liquid ratio 1g:15mL adds 300mL water to be sufficiently mixed, and is in frequency 40KHz, power are ultrasonic extraction 30min under 100W, the ul-trasonic irradiation that temperature is 70 DEG C, filter extract solution, collect to obtain filtrate;
(4) filtrate is carried out into freeze-drying by vacuum freeze drier, reclaims extractant-water, obtain golden camellia tea water Extract dry powder, obtains dry powder 2.66g, 2.68g, 2.44g, recovery rate analysis such as Fig. 6;
(5) by golden camellia tea dry composition into certain density solution to be measured, with catechin as standard items, standard curve is such as Fig. 7, is detected using vanillic aldehyde-concentrated hydrochloric acid development process to catechin content in extract, catechin content be 2.03mg/g, 1.88mg/g, 1.98mg/g, extract result statistics such as Fig. 8.
Embodiment 4
Using micro- method cut and help interaction technology to improve Camellia nitidissima extract catechin dissolution rate, with golden camellia tea as former Material, comprises the following steps:
(1) golden flower tea fresh leaves are taken, is cleaned, microwave high-temperature de-enzyme, vacuum condition is dried, then by dried golden camellia tea Crush, cross 60 mesh sieves, obtain golden camellia tea powder;
(2) the mesh powder 500g of golden camellia tea powder 60 is taken, 2% physics auxiliary agent 5g is added by mass percentage, is put into vibromill 10min is ground, micro- cutting is obtained and is helped powder, golden camellia tea grain diameter is shown in Fig. 1, golden camellia tea particulate scan electron microscope such as Fig. 5;
(3) take micro- the cutting of golden camellia tea and help powder 20g, by solid-liquid ratio 1g:15ml adds 300mL water to be sufficiently mixed, and is in frequency 40KHz, power are ultrasonic extraction 30min under 100W, the ul-trasonic irradiation that temperature is 70 DEG C, filter extract solution, collect to obtain filtrate;
(4) filtrate is carried out into freeze-drying by vacuum freeze drier, reclaims extractant-water, obtain golden camellia tea water Extract dry powder, obtains dry powder 3.74g, 3.78g, 3.84g, and 1.93 times, recovery rate analysis are improved compared with traditional extraction process Such as Fig. 6;
(5) by golden camellia tea dry composition into certain density solution to be measured, with catechin as standard items, standard curve is such as Fig. 7, is detected using vanillic aldehyde-concentrated hydrochloric acid development process to catechin content in extract, catechin content be 2.49mg/g, 2.51mg/g, 2.66mg/g, improve 4.59 times compared with traditional extraction process, extract result statistics such as Fig. 8.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any one skilled in the art in the technical scope of present disclosure, technology according to the present invention scheme and its Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.

Claims (3)

1. it is a kind of to cut the method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate with micro-, with golden camellia tea as former Material, it is characterised in that comprise the following steps:
S1, golden flower tea fresh leaves are taken, cleaned, de-enzyme dry, pulverize under vacuum condition, cross 60~200 mesh sieves, obtain golden camellia tea powder;
S2, by golden camellia tea powder obtained in step S1 and physics auxiliary agent by mass percentage 1:1%~4% grinding 10min, obtains micro- Cut and help powder;
The physics auxiliary agent is sharp property material;
S3, micro- cutting obtained in step S2 is helped into powder and water by solid-liquid ratio 1g:15mL is sufficiently mixed, ultrasound 30min at 70 DEG C, filtering Extract solution, collects to obtain filtrate;
The supersonic frequency is 40KHz, power is 100W;
S4, by the filtrate freeze-drying obtained by step S3, obtain golden camellia tea water extract dry powder.
2. the method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro- according to claim 1, its It is characterised by, the de-enzyme described in step S1 finishes for microwave high-temperature.
3. the method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro- according to claim 1, its It is characterised by, sharp property material described in step S2 is oyster shell whiting.
CN201710139512.XA 2017-03-10 2017-03-10 The method for helping interaction technology to improve Camellia nitidissima extract catechin dissolution rate is cut with micro- Pending CN106880699A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101485789A (en) * 2009-02-06 2009-07-22 广西桂人堂金花茶产业集团股份有限公司 Camellia chrysantha polysaccharide lozenge and method for producing the same
CN104383123A (en) * 2014-11-14 2015-03-04 程金生 Method for preparing golden camellia lipid-lowering blood sugar-reducing preparation
CN104958440A (en) * 2015-05-22 2015-10-07 大连理工大学 Camellia nitidissima Chi flower extract as well as preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101485789A (en) * 2009-02-06 2009-07-22 广西桂人堂金花茶产业集团股份有限公司 Camellia chrysantha polysaccharide lozenge and method for producing the same
CN104383123A (en) * 2014-11-14 2015-03-04 程金生 Method for preparing golden camellia lipid-lowering blood sugar-reducing preparation
CN104958440A (en) * 2015-05-22 2015-10-07 大连理工大学 Camellia nitidissima Chi flower extract as well as preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
罗昭润等: "金花茶的花茶与叶茶制作技术", 《福建农业科技》 *
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Application publication date: 20170623