CN110151869A - The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima - Google Patents

The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima Download PDF

Info

Publication number
CN110151869A
CN110151869A CN201910544707.1A CN201910544707A CN110151869A CN 110151869 A CN110151869 A CN 110151869A CN 201910544707 A CN201910544707 A CN 201910544707A CN 110151869 A CN110151869 A CN 110151869A
Authority
CN
China
Prior art keywords
camellia nitidissima
extraction
flavonoid substances
product
ethyl alcohol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910544707.1A
Other languages
Chinese (zh)
Inventor
周才碧
宋丽莎
周才元
王佳菜
刘丽明
石悦
周新
杨璐
陶旭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guizhou Bili Science And Technology Service Co Ltd
Qiannan Normal University for Nationalities
Original Assignee
Guizhou Bili Science And Technology Service Co Ltd
Qiannan Normal University for Nationalities
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guizhou Bili Science And Technology Service Co Ltd, Qiannan Normal University for Nationalities filed Critical Guizhou Bili Science And Technology Service Co Ltd
Priority to CN201910544707.1A priority Critical patent/CN110151869A/en
Publication of CN110151869A publication Critical patent/CN110151869A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • A61P39/06Free radical scavengers or antioxidants
    • 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
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH

Landscapes

  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Medicinal Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Epidemiology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a kind of techniques of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima.It is prepared: a, after drying Camellia nitidissima, being crushed as steps described below, low temperature seal saves, and obtains A product;B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 50-90%, A product and ethyl alcohol is 1:10-50gmL‑1, Extracting temperature is 40-90 DEG C, and extraction time 10-30min obtains Camellia nitidissima flavone extractive.The present invention has the Flavonoid substances recovery rate in Camellia nitidissima high, in Optimal technique process, the recovery rate of Camellia nitidissima Flavonoid substances is up to 5.41%, Camellia nitidissima Flavonoid substances increase the Scavenging activity of DPPH free radical and ABTS free radical, 74% and 84% are arrived separately at, the Scavenging activity of extract is strong, there is preferable oxidation resistance, so that Camellia nitidissima is widely developed and used, there are good economic benefit and social benefit.

Description

The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima
Technical field
The present invention relates to Flavonoid substances in a kind of Camellia nitidissima, flavones in especially a kind of ultrasonic wave assisted extraction Camellia nitidissima The technique of substance.
Background technique
Camellia nitidissima (Camellia chrysantha (Hu) Tuyama) belongs to Theaceae, Camellia Plants.Because it is with pole Its rare yellow coloration gene KNA, and it is known as " giant panda of plant kingdom ".Contain more Vitexin in Camellia nitidissima (vitesin), the Flavonoid substances such as Quercetin, Kaempferol, wherein based on Quercetin and kaempferol.Correlative study shows gold Jasmine tea leaf extract has obvious hypoglycemic and stronger removing hydroxyl radical free radical (OH), superoxide ion (O2) ability, and Effect is proportional to dosage.But the extraction of current Camellia nitidissima is substantially at the primary stage of research, and golden in the prior art Flavonoid substances recovery rate in jasmine tea is low, and the Scavenging activity of extract is poor, is unfavorable for the development and utilization of Camellia nitidissima.
In conclusion the prior art, there are the Flavonoid substances recovery rate in Camellia nitidissima is low, the Scavenging activity of extract is poor, The technical issues of being unfavorable for the development and utilization of Camellia nitidissima.
Summary of the invention
The object of the present invention is to provide a kind of techniques of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima.This hair It is bright high with the Flavonoid substances recovery rate in Camellia nitidissima, it is reached in the recovery rate of Optimal technique process, Camellia nitidissima Flavonoid substances 5.41%, Camellia nitidissima Flavonoid substances increase the Scavenging activity of DPPH free radical and ABTS free radical, have arrived separately at 74% With 84%, the Scavenging activity of extract is strong, there is preferable oxidation resistance, so that Camellia nitidissima is widely developed and used, has Good economic benefit and social benefit.
Technical solution of the present invention: the technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima, according to following It is prepared by step:
A, it by after Camellia nitidissima drying, crushes, low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 50-90%, A product and ethyl alcohol is 1:10-50g·mL-1, Extracting temperature is 40-90 DEG C, and extraction time 10-30min obtains Camellia nitidissima flavone extractive.
It is by Camellia nitidissima in the step a in ultrasonic wave assisted extraction Camellia nitidissima above-mentioned in the technique of Flavonoid substances In 100-110 DEG C of drying box after dry 20-40min, 50-70 mesh is crushed in ultrahigh speed pulverizer, the low temperature at 3-5 DEG C It is sealed;It prevents Flavonoid substances in Camellia nitidissima tealeaves from aoxidizing by low temperature seal preservation, and prevents aqueous vapor mould into causing Become.
It is by Camellia nitidissima in the step a in ultrasonic wave assisted extraction Camellia nitidissima above-mentioned in the technique of Flavonoid substances In 105 DEG C of drying boxes after dry 30min, 60 mesh are crushed in ultrahigh speed pulverizer, low temperature seal saves at 4 DEG C.
In ultrasonic wave assisted extraction Camellia nitidissima above-mentioned in the technique of Flavonoid substances, in the step b, A product are used The material ratio of ethyl alcohol progress ultrasonic extraction, volume fraction of ethanol 53-80%, A product and ethyl alcohol is 1:12-40gmL-1, extract Temperature is 50-87 DEG C, extraction time 22-28min.
In ultrasonic wave assisted extraction Camellia nitidissima above-mentioned in the technique of Flavonoid substances, in the step b, A product are used The material ratio of ethyl alcohol progress ultrasonic extraction, volume fraction of ethanol 55-70%, A product and ethyl alcohol is 1:15-30gmL-1, extract Temperature is 60-85 DEG C, extraction time 23-27min.
In ultrasonic wave assisted extraction Camellia nitidissima above-mentioned in the technique of Flavonoid substances, in the step b, A product are used The material ratio of ethyl alcohol progress ultrasonic extraction, volume fraction of ethanol 60%, A product and ethyl alcohol is 1:20gmL-1, Extracting temperature is 80 DEG C, extraction time 25min.
Compared with prior art, the present invention is by having the advantages that
1, the technology also prematurity in Camellia nitidissima in terms of Flavonoid substances is extracted at present, and the present invention is extracted using organic solvent Method carries out the single factor experiments such as volume fraction of ethanol, extraction time, Extracting temperature, material ratio and optimization of orthogonal test design, It is intended to probe into Flavonoid substances optimum extraction process and antioxidation activity in vitro in Camellia nitidissima, to be Camellia nitidissima development and utilization Certain reference is provided.
2, Orthogonal experiment results of the invention explanation, influence of the different factors to Camellia nitidissima extracting flavonoids rate is: ethyl alcohol Volume fraction > Extracting temperature > material ratio > extraction time, i.e. ultrasonic wave assisted extraction method extract Camellia nitidissima Flavonoid substances most Excellent process conditions are as follows: volume fraction of ethanol 60%, Extracting temperature are 80 DEG C, material ratio 1:20gmL-1, extraction time is 25min, with this condition, the recovery rates of Camellia nitidissima Flavonoid substances is up to 5.41%.
3, Camellia nitidissima chromocor extract of the invention removes ABTS free radical ability lower than VC, but its clearance rate is dense with flavones The increase of degree and increase, and it is more etc. to be better than Lee] pass through the quinoa chaff chromocor extract of ultrasonic wave extraction, it is seen that its still show compared with Strong Scavenging activity.In addition, antioxidation in vitro experiment shows: with the raising of Camellia nitidissima general flavone concentration, to DPPH freedom The Scavenging activity of base and ABTS free radical increases, and has arrived separately at 74% and 84%.
4, with the continuous enhancing of the increasingly raising and health care consciousness of people's living standard, using Camellia nitidissima as raw material, from gold Flavones is extracted in jasmine tea, not only can satisfy on contemporary medical science, food additives and cosmetics are to the needs of flavones, but also make gold Jasmine tea is widely developed and used, therefore the technical study for probing into tealeaves is with good economic efficiency and social benefit.And The extraction of Camellia nitidissima is substantially at the primary stage of research at present;Therefore the extraction to Camellia nitidissima Flavonoid substances is needed to enter depth The research entered makes great efforts to improve yield and efficiency, and realization moves towards production reality from laboratory, makes Camellia nitidissima in the national warp of development Ji promotes to play positive effect in human health.
Inventor has carried out following experiment:
1 experiment purpose
Using organic solvent leach extraction method, the Dan Yin such as volume fraction of ethanol, extraction time, Extracting temperature, material ratio are carried out Element test and optimization of orthogonal test design, it is intended in probing into Flavonoid substances optimum extraction process and antioxidation in vitro in Camellia nitidissima Activity, to provide certain reference for Camellia nitidissima development and utilization.
2 materials and methods
2.1 test material
2.1.1 raw material
Camellia nitidissima tealeaves: it adopts in Guizhou Duyun City Luodian County
2.1.2 reagent
Dehydrated alcohol, aluminum nitrate, sodium hydroxide, sodium nitrite etc. are that analysis is pure;Rutin standard items, purity >=98%; DPPH, Sigma;ABTS, Sigma.
2.1.3 instrument
(1) ultraviolet specrophotometer: UV5200, Shanghai instrument electric analysis Instrument company;
(2) sonic washing machine: hypersonic sound instrument company is preced in SG2200HPT, Shanghai;
(4) other instruments: electronic analytical balance, tea pulverizer, volumetric flask (100mL, 50mL10mL), conical flask (200mL), liquid-transfering gun etc..
2.2 test method
2.2.1 sample preparation
Purchased Camellia nitidissima is dried into 30min in 105 DEG C of drying boxes, 60 mesh are crushed in ultrahigh speed pulverizer, in 4 DEG C It is saved backup in low temperature seal environment.
2.2.2 sample detection
(1) drafting of standard curve: regression analysis is carried out with concentration X and Y, obtains regression equation y=5.3771x+0.0280.
(2) it the extraction of Flavonoid substances: weighs golden flower tea powder 2.000g (m) and is placed in the vial with cover of 200mL, press According to table 2.1, ultrasonic extraction is carried out to Camellia nitidissima, Camellia nitidissima flavone extractive is filtered to 100mL (V1) in volumetric flask, 70% C2H5OH is settled to graduation mark, shakes up spare.
Take 1mL (V2) Camellia nitidissima flavone extractive is in 10mL (V3) in volumetric flask, reagent needed for being added measures absorbance A510nm, same measurement designs 3 parallel tests, is averaged, finds out flavones yield, formula is as follows:
TRecovery rate(%)=(X × V1×V3)/(V2×m×10)
2.2.3 single factor experiment
2.1 single factor experiment scheme of table
Golden flower tea powder 2.000g is taken, studies extraction time (10,15,20,25,30min) respectively, Extracting temperature (40, 50,60,70,80 DEG C), volume fraction of ethanol (50%, 60%, 70%, 80%, 90%), material ratio (1:10,1:20,1:30, 1:40、1:50)g·mL-1To the influence that Camellia nitidissima Flavonoid substances extract, see Table 2 for details .1.
2.2.4 orthogonal test
Referring to 2.2 factor level of table, using L9(34) orthogonal trial, Camellia nitidissima Flavonoid substances recovery rate is investigated, is obtained Optimal extract process, same measurement design 3 parallel tests, are averaged.
2.2 orthogonal test factor level of table designs table
2.2.5 Camellia nitidissima Flavonoid substances antioxidation in vitro is studied
(1) DPPH Scavenging activity measures: taking 2 × 10-4The DPPH solution of mol/L, is separately added into the Camellia nitidissima of various concentration Flavone extractive shakes up, and 30min is placed in no light conditions.Measure light absorption value A1(517nm) and flavone extractive and water Light absorption value A2, then measure the light absorption value A of DPPH solution0.Calculation is as follows:
DPPH free radical scavenging activity (%)=[1- (A1-A2)/A0]×100
(2) ABTS Scavenging activity measures: the flavone extractive of various concentration is drawn, ABTS working solution is added and shakes up, in Light absorption value A is measured at 734nm1, blank absorbency A is made with ABTS working solution and water0, Camellia nitidissima flavone extractive mixes with water Even absorbance is A2.It calculates as follows:
ABTS free radical scavenging activity (%)=[1- (A1-A2)/A0]×100
The analysis of 2.3 data
For statistical analysis to data using SAS9.2 software, all data are indicated with x ± Std, and P > 0.05 indicates poor Different not significant, 0.01 < P < 0.05 indicates that significant difference, P < 0.01 indicate that difference is extremely significant;The mapping of Origin9.0 software.
3 results and analysis
3.1 simple experiment variance analyses
3.1.1 influence of the extraction time to extracting flavonoids rate in Camellia nitidissima
3.1 significance analysis table of table
Known according to table 3.1, different extraction times are to the F statistic of Flavonoid substances recovery rate difference in Camellia nitidissima tealeaves 241.1, P values are < 0.0001, greater than the F value in 0.01 level, it is known that different extraction times are to extracting flavonoids rate in Camellia nitidissima Influence have highly significant difference.
Extracting flavonoids rate in Camellia nitidissima is influenced by Fig. 1 different extraction time Multiple range test it is found that 0.01 level On, processing 3 has extremely significant difference with processing 1,2,4,5, and influence of the different extraction times to extracting flavonoids rate in Camellia nitidissima is Processing 3 > processing 2 > processing 4 > processing 1 > processing 5;For the extracting flavonoids rate of Camellia nitidissima, processing 3 at most, is followed by handled 2, and the two has extremely significance difference anisotropic;The influence for comprehensively considering extracting flavonoids rate in 3 pairs of Camellia nitidissimas of processing is optimal, it may be assumed that extracts Temperature 60 C, material ratio 1:30gmL-1, extraction time 20min, ethyl alcohol volume be 70%, Flavonoid substances recovery rate reaches 4.463%.
3.1.2 influence of the Extracting temperature to extracting flavonoids rate in Camellia nitidissima
3.2 significance analysis table of table
Known according to table 3.2, different Extracting temperatures are 262.57, P value to the F statistic of extracting flavonoids rate difference in Camellia nitidissima It is < 0.0001, greater than the F value in 0.01 level, it is known that influence of the different Extracting temperatures to extracting flavonoids rate in Camellia nitidissima has Highly significant difference.
By Fig. 2 difference Extracting temperature in Camellia nitidissima extracting flavonoids rate influence Multiple range test it is found that 0.01 level On, processing 3 has extremely significant difference with processing 1,2,4,5, and influence of the different Extracting temperatures to extracting flavonoids rate in Camellia nitidissima is Processing 3 > processing 2 > processing 4 > processing 1 > processing 5;For the extracting flavonoids rate of Camellia nitidissima, processing 3 at most, is followed by handled 2, and the two has extremely significance difference anisotropic;The influence for comprehensively considering extracting flavonoids rate in 3 pairs of Camellia nitidissimas of processing is optimal, it may be assumed that material Compare 1:30gmL-1, 60 DEG C of Extracting temperature, extraction time 60min, ethyl alcohol volume be 70%, extracting flavonoids rate reaches 5.849%.
3.1.3 influence of the ethyl alcohol volume to extracting flavonoids rate in Camellia nitidissima
3.3 significance analysis table of table
Known according to table 3.3, different ethyl alcohol volumes are 705.23, P value to the F statistic of extracting flavonoids rate difference in Camellia nitidissima It is < 0.0001, greater than the F value in 0.01 level, it is known that influence of the different ethyl alcohol volumes to extracting flavonoids rate in Camellia nitidissima has Highly significant difference.
By Fig. 3 difference ethyl alcohol volume in Camellia nitidissima extracting flavonoids rate influence Multiple range test it is found that 0.01 level On, processing 5 has extremely significant difference with processing 1,2,3,4, and influence of the different ethyl alcohol volumes to extracting flavonoids rate in Camellia nitidissima is Processing 3 > processing 2 > processing 4 > processing 1 > processing 5;For the extracting flavonoids rate of Camellia nitidissima, processing 3 at most, is followed by handled 2, and the two has extremely significance difference anisotropic;The influence for comprehensively considering extracting flavonoids rate in 3 pairs of Camellia nitidissimas of processing is optimal, it may be assumed that ethyl alcohol Volume 70%, material ratio 1:30gmL-1, 60 DEG C of Extracting temperature, extraction time 20min, extracting flavonoids rate reaches 4.587%.
3.1.4 influence of the material ratio to extracting flavonoids rate in Camellia nitidissima
3.4 significance analysis table of table
Known according to table 3.4, different material compare the F statistic of extracting flavonoids rate difference in Camellia nitidissima be 872.6, P value for < 0.0001, greater than the F value in 0.01 level, it is known that the influence that different material compares extracting flavonoids rate in Camellia nitidissima has extremely aobvious The difference of work.
By the Multiple range test of extracting flavonoids rate influence in Fig. 4 different material comparison Camellia nitidissima it is found that in 0.01 level, Processing 1 has an extremely significant difference with processing 2,3,4,5, different material compare extracting flavonoids rate in Camellia nitidissima influence be processing 3 > Processing 4 > processing 2 > processing 5 > processing 1;For the extracting flavonoids rate of Camellia nitidissima, processing 3 at most, followed by handles 4, and two Person has extremely significance difference anisotropic;The influence for comprehensively considering extracting flavonoids rate in 3 pairs of Camellia nitidissimas of processing is optimal, it may be assumed that material ratio 1: 30g·mL-1, 60 DEG C of Extracting temperature, extraction time 60min, ethyl alcohol volume be 70%, extracting flavonoids rate reaches 5.058%.
3.2 orthogonal test variance analyses
3.5 orthogonal experiments of table
On the basis of above-mentioned experiment, using general flavone recovery rate as inspection target, L is carried out9(34) orthogonal test, factor water It puts down as shown in table 2.2, orthogonal experiments and data analysis are shown in Table 3.5.
Orthogonal experiment results explanation, influence of the different factors to Camellia nitidissima extracting flavonoids rate is: volume fraction of ethanol > mention Take temperature > material ratio > extraction time, optimum process condition A2B3C1D3, i.e. volume fraction of ethanol is 60%, and Extracting temperature is 80 DEG C, material ratio 1:20gmL-1, extraction time 25min.
The research of 3.3 Camellia nitidissima flavones antioxidation in vitro
3.3.1 DPPH free radical scavenging ability
By Fig. 5 DPPH free radical scavenging activity it is found that Flavonoid substances are obviously low to DPPH free radical scavenging activity in Camellia nitidissima In VC, this may be that the extract is mixture, and purity is low, impurity is more, it is suppressed that its activity;But its clearance rate is with concentration Increase and constantly increase, can reach 74%, illustrate in Camellia nitidissima that Flavonoid substances have preferable antioxidant activity.
3.3.2 ABTS free radical scavenging ability
By Fig. 6 ABTS free radical scavenging activity it is found that Camellia nitidissima chromocor extract, which removes ABTS free radical ability, is lower than VC, but Its clearance rate increases with the increase of flavonoid concentration, can reach 84%, and is better than the mostly equal quinoa chaff by ultrasonic wave extraction of Lee Chromocor extract, it is seen that it still shows stronger Scavenging activity.
4.1 discussing
Single factor experiment the result shows that, in 60 DEG C of Extracting temperature, material ratio 1:30gmL-1, volume fraction of ethanol 70% Under the conditions of, the Camellia nitidissima flavones optimum extraction time is 20min, and recovery rate reaches 4.463%;20min, material ratio between at the extraction 1:30g·mL-1, under conditions of volume fraction of ethanol 70%, Camellia nitidissima flavones optimum extraction temperature is 60 DEG C, and recovery rate reaches 5.849%;20min, 60 DEG C of Extracting temperature, material ratio 1:30gmL between at the extraction-1Under conditions of, Camellia nitidissima flavones is best Volume fraction of ethanol is 70%, and recovery rate reaches 4.587%;20min, 60 DEG C of Extracting temperature, ethyl alcohol volume point between at the extraction Under conditions of number 70%, the best material ratio of Camellia nitidissima flavones is 1:30gmL-1, recovery rate reaches 5.058%.
Orthogonal experiments show the influence factor sequence to Camellia nitidissima extracting flavonoids rate are as follows: volume fraction of ethanol > extraction Temperature > material ratio > extraction time.
4.2 conclusion
Extracting the brown sugar substance in Camellia nitidissima using ultrasonic wave assisted extraction method has good effect, ultrasonic wave auxiliary The Optimal technique process of extraction method extraction Camellia nitidissima Flavonoid substances are as follows: volume fraction of ethanol 60%, Extracting temperature are 80 DEG C, Material ratio is 1:20gmL-1, extraction time 25min, with this condition, the recovery rate of Camellia nitidissima Flavonoid substances reach 5.41%.And Camellia nitidissima flavones becomes by force the Scavenging activity of DPPH free radical, ABTS free radical with the raising of concentration, says It is bright its with preferable oxidation resistance.
In conclusion the present invention has the Flavonoid substances recovery rate in Camellia nitidissima high, in Optimal technique process, Camellia nitidissima The recovery rate of Flavonoid substances is up to 5.41%, Scavenging activity of the Camellia nitidissima Flavonoid substances to DPPH free radical and ABTS free radical Increase, has arrived separately at 74% and 84%, the Scavenging activity of extract is strong, has preferable oxidation resistance, so that Camellia nitidissima obtains To extensive development and utilization, there is the beneficial effect of good economic benefit and social benefit.
Detailed description of the invention
Fig. 1 is the Multiple range test influenced on extracting flavonoids rate in Camellia nitidissima different extraction times of the invention;
Fig. 2 is the Multiple range test that different Extracting temperatures of the invention influence extracting flavonoids rate in Camellia nitidissima;
Fig. 3 is the Multiple range test that different ethyl alcohol volumes of the invention influence extracting flavonoids rate in Camellia nitidissima;
Fig. 4 is the Multiple range test that different material of the invention compares that extracting flavonoids rate influences in Camellia nitidissima;
Fig. 5 is the DPPH free radical scavenging activity of Flavonoid substances in Camellia nitidissima of the present invention;
Fig. 6 is the ABTS free radical scavenging activity of Flavonoid substances in Camellia nitidissima of the present invention.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment 1.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 20min, is crushed to 50 mesh, at 3 DEG C in 100 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 50%, A product and ethyl alcohol is 1: 10g·mL-1, Extracting temperature is 40 DEG C, and extraction time 10min obtains Camellia nitidissima flavone extractive.
Embodiment 2.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 30min, is crushed to 60 mesh, at 4 DEG C in 105 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 60%, A product and ethyl alcohol is 1: 20g·mL-1, Extracting temperature is 50 DEG C, and extraction time 23min obtains Camellia nitidissima flavone extractive.
Embodiment 3.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 20min, is crushed to 70 mesh, at 3 DEG C in 110 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 70%, A product and ethyl alcohol is 1: 30g·mL-1, Extracting temperature is 60 DEG C, and extraction time 25min obtains Camellia nitidissima flavone extractive.
Embodiment 4.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 40min, is crushed to 50 mesh, at 5 DEG C in 100 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 80%, A product and ethyl alcohol is 1: 40g·mL-1, Extracting temperature is 70 DEG C, and extraction time 28min obtains Camellia nitidissima flavone extractive.
Embodiment 5.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 30min, is crushed to 60 mesh, at 4 DEG C in 105 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 60%, A product and ethyl alcohol is 1: 20g·mL-1, Extracting temperature is 80 DEG C, and extraction time 25min obtains Camellia nitidissima flavone extractive.
Embodiment 6.The technique of Flavonoid substances, is made as steps described below in a kind of ultrasonic wave assisted extraction Camellia nitidissima It is standby:
A, Camellia nitidissima after dry 40min, is crushed to 70 mesh, at 5 DEG C in 110 DEG C of drying boxes in ultrahigh speed pulverizer Lower low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 90%, A product and ethyl alcohol is 1: 50g·mL-1, Extracting temperature is 90 DEG C, and extraction time 30min obtains Camellia nitidissima flavone extractive.

Claims (6)

1. the technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima, it is characterised in that: carry out as steps described below Preparation:
A, it by after Camellia nitidissima drying, crushes, low temperature seal saves, and obtains A product;
B, A product are subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 50-90%, A product and ethyl alcohol is 1: 10-50g·mL-1, Extracting temperature is 40-90 DEG C, and extraction time 10-30min obtains Camellia nitidissima flavone extractive.
2. the technique of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima according to claim 1, it is characterised in that: institute It states in step a, is after dry 20-40min, to be crushed to Camellia nitidissima in ultrahigh speed pulverizer in 100-110 DEG C of drying box 50-70 mesh, low temperature seal saves at 3-5 DEG C.
3. the technique of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima according to claim 2, it is characterised in that: institute It states in step a, is that Camellia nitidissima after dry 30min, is crushed to 60 mesh, 4 in 105 DEG C of drying boxes in ultrahigh speed pulverizer Low temperature seal saves at DEG C.
4. the technique of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima according to claim 1, it is characterised in that: institute It states in step b, A product is subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 53-80%, A product and ethyl alcohol is 1:12-40g·mL-1, Extracting temperature is 50-87 DEG C, extraction time 22-28min.
5. the technique of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima according to claim 4, it is characterised in that: institute It states in step b, A product is subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 55-70%, A product and ethyl alcohol is 1:15-30g·mL-1, Extracting temperature is 60-85 DEG C, extraction time 23-27min.
6. the technique of Flavonoid substances in ultrasonic wave assisted extraction Camellia nitidissima according to claim 5, it is characterised in that: institute It states in step b, A product is subjected to ultrasonic extraction using ethyl alcohol, the material ratio of volume fraction of ethanol 60%, A product and ethyl alcohol is 1: 20g·mL-1, Extracting temperature is 80 DEG C, extraction time 25min.
CN201910544707.1A 2019-06-21 2019-06-21 The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima Pending CN110151869A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910544707.1A CN110151869A (en) 2019-06-21 2019-06-21 The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910544707.1A CN110151869A (en) 2019-06-21 2019-06-21 The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima

Publications (1)

Publication Number Publication Date
CN110151869A true CN110151869A (en) 2019-08-23

Family

ID=67626652

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910544707.1A Pending CN110151869A (en) 2019-06-21 2019-06-21 The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima

Country Status (1)

Country Link
CN (1) CN110151869A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114904294A (en) * 2022-06-28 2022-08-16 闽江师范高等专科学校 Preparation method of high-yield tea flavone

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106511625A (en) * 2016-12-05 2017-03-22 东兴鑫宇实业有限公司 Ultrasonic extraction method of camellia nitidissima flavone

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106511625A (en) * 2016-12-05 2017-03-22 东兴鑫宇实业有限公司 Ultrasonic extraction method of camellia nitidissima flavone

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张佩霞: "金花茶黄酮类化合物的生物学功能及提取分离测定方法研究进展", 《广东农业科学》 *
李石容: "金花茶茶花黄酮类化合物的分离纯化及抗氧化活性的初步研究", 《中国优秀硕士学位论文全文数据库 农业科技辑》 *
牛广俊: "基于抗氧化活性优化金花茶花超声提取工艺", 《福建林业科技》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114904294A (en) * 2022-06-28 2022-08-16 闽江师范高等专科学校 Preparation method of high-yield tea flavone

Similar Documents

Publication Publication Date Title
Jiang et al. Extraction of water-soluble polysaccharide and the antioxidant activity from Ginkgo biloba leaves
CN105998109A (en) Mango seed polyphenol extract and preparation method thereof
CN108815036A (en) A kind of preparation method and applications of Ta Naka extract
CN104000892A (en) Method for extracting peony general flavone from peonies
CN104987427A (en) Complex enzyme microwave extraction method for optimizing lycium ruthenicum polysaccharide by utilizing response surface method
CN108250320B (en) Low-ash ganoderma lucidum polysaccharide extract and preparation method thereof
CN110013493A (en) The extraction process of the kusamaki broad-leaved podocarpus seed and receptacle flavones of response phase method optimization
CN102816637B (en) Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids
CN112168873B (en) Extraction process for optimizing total flavonoids of Cotoneaster horizontalis by response surface method
CN103110674B (en) Nitraria tangutorum bobr total phenolic extract, as well as extraction method and application thereof
CN104059160B (en) A kind of Hericium erinaceus (Bull. Ex Fr.) Pers. cell wall polysaccharides and preparation method thereof
CN110151869A (en) The technique of Flavonoid substances in a kind of ultrasonic wave assisted extraction Camellia nitidissima
CN103766913B (en) A kind of method extracting total stilbene compound from seed of Flos Moutan
CN103705647A (en) Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method
CN107929326A (en) A kind of American-cockroach-extract, preparation method and its application in anti-oxidant adjusting
CN107375503A (en) The preparation method of soapberry pericarp activity extract and its antimycotic application
CN104586904B (en) A kind of separated in synchronization prepares cynomorium songaricum polysaccharide and the method for cynomorium songaricum flavones
CN114469790B (en) Method for preparing water-soluble poria cocos sclerotium extract
CN106138130A (en) A kind of mango core chromocor extract and preparation method thereof
CN104109180A (en) Compound having antioxidant activity and application
CN109771475A (en) A method of extracting polyphenol from purple perilla seed shell
CN106666707B (en) Preparation method and application of Sipunculus nudus antioxidant extract
Konieczynski Principal component analysis in interpretation of the results of HPLC-ELC, HPLC-DAD and essential elemental contents obtained for medicinal plant extracts
CN106214799B (en) A kind of extracting method of orange peel general flavone
CN107619422A (en) A kind of method for preparing the O glucuronides of high-purity gossypitrin 8

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190823