CN110156604A - A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid - Google Patents
A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid Download PDFInfo
- Publication number
- CN110156604A CN110156604A CN201910541341.2A CN201910541341A CN110156604A CN 110156604 A CN110156604 A CN 110156604A CN 201910541341 A CN201910541341 A CN 201910541341A CN 110156604 A CN110156604 A CN 110156604A
- Authority
- CN
- China
- Prior art keywords
- chlorogenic acid
- water
- value
- yellow fruit
- recovery rate
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F17/00—Digital computing or data processing equipment or methods, specially adapted for specific functions
- G06F17/10—Complex mathematical operations
- G06F17/18—Complex mathematical operations for evaluating statistical data, e.g. average values, frequency distributions, probability functions, regression analysis
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F30/00—Computer-aided design [CAD]
- G06F30/20—Design optimisation, verification or simulation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Theoretical Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Data Mining & Analysis (AREA)
- General Engineering & Computer Science (AREA)
- Pure & Applied Mathematics (AREA)
- Mathematical Analysis (AREA)
- Mathematical Optimization (AREA)
- Computational Mathematics (AREA)
- Mathematical Physics (AREA)
- Databases & Information Systems (AREA)
- Algebra (AREA)
- Probability & Statistics with Applications (AREA)
- Evolutionary Biology (AREA)
- Software Systems (AREA)
- Operations Research (AREA)
- Bioinformatics & Computational Biology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Computer Hardware Design (AREA)
- Evolutionary Computation (AREA)
- Geometry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid, belong to technical field of plant extraction.The following steps are included: carrying out refluxing extraction after yellow fruit eggplant sample powder is mixed with water, the pH value of the water is 2~11.The present invention with cleanliness without any pollution, saves the considerable advantage of economic cost using water as the extraction of Extraction solvent progress yellow fruit eggplant Content of Chlorogenic Acid, while passing through the pH value for limiting water, improves recovery rate, while is improved industrialization efficiency also.Embodiment statistics indicate that, the optimum extraction process of yellow fruit eggplant Content of Chlorogenic Acid of the present invention is: using water as extractant, liquid-to-solid ratio 50mL:1g, 90 DEG C of temperature, the pH value of water is 2, time 1h, the recovery rate maximum 0.28% of chlorogenic acid, different technology conditions to the influence degree of chlorogenic acid yield from big to small are as follows: time > pH value > temperature > liquid-to-solid ratio.
Description
Technical field
The present invention relates to technical field of plant extraction more particularly to a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid.
Background technique
Yellow fruit eggplant (Fruit of yellowfruit nightshade) is a kind of common Chinese medicine, is had a very wide distribution,
The ground such as Yunnan, Fujian, Guangxi, Sichuan are distributed mainly on, the area of the arid such as rural area roadside, wasteland is grown in.Contain in yellow fruit eggplant
Having can be with the natural organic acids of the multiple efficacies such as blood fat-reducing blood pressure-decreasing, antitumor.Alkaloid is related generally to the research of yellow fruit eggplant at present
The research of aspect.
Chlorogenic acid (Chlorogenic acid) is caffeic acid (Caffeic acid) and chinic acid (Quinic acid) contracting
A kind of styrene acrylic compound, is present in the fruit and leaf of dicotyledon more made of conjunction, such as fructus arctii, honeysuckle, yellow fruit eggplant
Deng.The molecular formula of chlorogenic acid is C16H18O9, relative molecular mass 354.31,665 DEG C of boiling point, white crystalline body is soluble in second
Alcohol, acetone, insoluble in organic solvents such as ether, chloroform, ethyl acetate.Nineteen eighty-two has determined the chemical structure such as formula 1 of chlorogenic acid
It is shown:
Chlorogenic acid is a kind of natural organic acid, has the function of antitumor, antibacterial, antiviral, anti-oxidant, reducing blood sugar and blood lipid
Deng.At present wide application daily cosmetics and in terms of.
It is many to the extracting method of chlorogenic acid in the prior art, mainly there are soxhlet extraction method, ultrasound on extracting method, water to mention
Method, normal reflux extraction method, alcohol extracting method, enzymatic isolation method, water extraction and alcohol precipitation method, water-boiling method, warm leaching method etc., traditional extracting method has
The shortcomings that recovery rate is low and industrializes low efficiency.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid.The present invention provides
Extracting method recovery rate is high, industrialization is high-efficient.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid, comprising the following steps:
Refluxing extraction is carried out after yellow fruit eggplant sample powder is mixed with water, the pH value of the water is 2~11.
Preferably, the pH value of the water is 2~3.
Preferably, the liquid-to-solid ratio of the water and yellow fruit eggplant sample powder is 20~70mL:1g.
Preferably, the temperature of the refluxing extraction is 40~90 DEG C.
Preferably, the time of the refluxing extraction is 0.5~3h.
Preferably, the time of the refluxing extraction is 1.5~2h.
Preferably, the temperature of the refluxing extraction is 90 DEG C, time 1h, and water and the liquid-to-solid ratio of yellow fruit eggplant sample powder are
50mL:1g, the pH value of water are 2.
Preferably, the temperature of the refluxing extraction is 80 DEG C, time 1.5h, the liquid-to-solid ratio of water and yellow fruit eggplant sample powder
For 40mL:1g, the pH value of water is 4.
Preferably, the yellow fruit eggplant sample powder sieves with 100 mesh sieve.
Preferably, the place of production of the yellow fruit eggplant sample powder includes Pu'er Simao, Red River Geju City, Qujing Luoping, Qujing teacher
Ancestor, Chuxiong Wuding County, Pu'er Jing Dong, Kunming Xun Dian or mountain of papers Maguan.
The present invention provides a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid, comprising the following steps: by yellow fruit eggplant sample powder
End carries out refluxing extraction after mixing with water, the pH value of the water is 2~11.The present invention carries out in yellow fruit eggplant by Extraction solvent of water
The extraction of chlorogenic acid with cleanliness without any pollution, saves the considerable advantage of economic cost, while passing through the pH value of restriction water, raising
Recovery rate, while making to industrialize efficiency and also be improved.
Further, the present invention is optimized extraction conditions by response phase method, has searched out a kind of optimal mention
Taking technique, response surface optimization method (Response Surface Methodology, RSM) they are to utilize mathematical modeling, reasonable group
Test design method is closed, certain required data are obtained by experiment, using polynary quadratic regression equation come data fitting and response
Relationship between value analyzes required data, seeks optimal procedure parameters to the analysis of regression equation, solves multivariable
A kind of statistical method of problem.This method is with intuitive is strong, estimated performance is good, high accuracy for examination.The data of embodiment
Showing the optimum extraction process of yellow fruit eggplant Content of Chlorogenic Acid of the present invention is: using water as extractant, liquid-to-solid ratio 50mL:1g, and temperature 90
DEG C, the pH value of water is 2, time 1h, the recovery rate maximum 0.28% of chlorogenic acid, shadow of the different technology conditions to chlorogenic acid yield
The degree of sound is from big to small are as follows: time > pH value > temperature > liquid-to-solid ratio.
Detailed description of the invention
Fig. 1 is the abosrption spectrogram of chlorogenic acid titer；
Fig. 2 is the standard curve of chlorogenic acid titer；
Fig. 3 is extraction efficiency figure of the different extractants to chlorogenic acid；
Fig. 4 is influence curve of the liquid-to-solid ratio to yellow fruit eggplant chlorogenic acid yield；
Fig. 5 is influence curve of the temperature to yellow fruit eggplant chlorogenic acid yield；
Fig. 6 is influence curve of the pH value to yellow fruit eggplant chlorogenic acid yield；
Fig. 7 is influence curve of the time to yellow fruit eggplant chlorogenic acid yield；
Fig. 8 is the influence contour map of temperature and liquid-to-solid ratio to recovery rate；
Fig. 9 is the influence diagram of temperature and liquid-to-solid ratio to recovery rate；
Figure 10 is the influence contour map of temperature and pH value to recovery rate；
Figure 11 is the influence of temperature and pH value to recovery rate；
Figure 12 is influence contour map of the temperature and time to recovery rate；
Figure 13 is influence of the temperature and time to recovery rate；
Figure 14 is the influence contour map of liquid-to-solid ratio and pH value to recovery rate；
Figure 15 is the influence of liquid-to-solid ratio and pH value to recovery rate；
Figure 16 is the influence contour map of liquid-to-solid ratio and time to recovery rate；
Figure 17 is the influence of liquid-to-solid ratio and time to recovery rate；
Figure 18 is the influence contour map of pH value and time to recovery rate；
Figure 19 is the influence of pH value and time to recovery rate.
Specific embodiment
The present invention provides a kind of extracting methods of yellow fruit eggplant Content of Chlorogenic Acid, comprising the following steps:
Refluxing extraction is carried out after yellow fruit eggplant sample powder is mixed with water, the pH value of the water is 2~11.
In the present invention, the pH value of the water is preferably 2~3.
In the present invention, the liquid-to-solid ratio of the water and yellow fruit eggplant sample powder is preferably 20~70mL:1g.
In the present invention, the yellow fruit eggplant sample powder preferably sieves with 100 mesh sieve.
In the present invention, the temperature of the refluxing extraction is preferably 40~90 DEG C.
In the present invention, the time of the refluxing extraction is preferably 0.5~3h, more preferably 1.5~2h.
In one embodiment of the invention, the refluxing extraction parameter preferably includes: temperature is 90 DEG C, time 1h,
The liquid-to-solid ratio of water and yellow fruit eggplant sample powder is 50mL:1g, and the pH value of water is 2.The present invention is 2 to the pH value for realizing water
Mode is not specifically limited.
In one embodiment of the invention, the refluxing extraction parameter preferably includes: temperature is 80 DEG C, and the time is
The liquid-to-solid ratio of 1.5h, water and yellow fruit eggplant sample powder is 40mL:1g, and the pH value of water is 4.The present invention is to the pH value for realizing water
It is not specifically limited for 4 mode.
In the present invention, the place of production of the yellow fruit eggplant sample powder preferably includes Pu'er Simao, Red River Geju City, Qujing sieve
Flat, Qujing master of great learning and integrity, Chuxiong Wuding County, Pu'er Jing Dong, Kunming Xun Dian or mountain of papers Maguan.
In order to further illustrate the present invention, below with reference to example to the extraction side of yellow fruit eggplant Content of Chlorogenic Acid provided by the invention
Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Yellow fruit solanberry picks up from Yunnan Province 8 Tonzhou Ge Bu county (Puer City Simao, Puer City Jing Dong, Qujing Luoping County, song in fact
The Shizong County Jing Shi, Honghe Geju City county, the Kunming county Xun Dian, Wenshan Prefecture Maguan County, Chuxiong Prefecture Wuding county), it dries, crushes, mistake
100 meshes, are sealed；Chlorogenic acid standard items are purchased from Hefei Bo Mei biotechnology Co., Ltd；Ethyl alcohol, methanol, acetone,
Hydrochloric acid, sodium hydroxide are analytical reagents.
Shimadzu UV-2550 ultraviolet-visible spectrophotometer, (ancient cooking vessel prosperous suitable experimental facilities in Shenzhen's has HH-6 thermostat water bath
Limit company), FA3204B electronic balance (upper Nereid Ke Tianmei balance equipment factory)
The preparation of chlorogenic acid standard solution
Weigh chlorogenic acid standard items 5.0mg, precision weighing is placed in 100mL volumetric flask, continuously add 70% ethyl alcohol it is molten
Solution, constant volume shake up for use, and concentration is 50 μ g/mL at this time.
The determination of maximum absorption wavelength
Take chlorogenic acid titer 20mL in the volumetric flask of 50mL, with 70% ethyl alcohol constant volume, under ultraviolet specrophotometer
It is scanned in 200nm~500nm wave-length coverage, as a result such as Fig. 1.Occurs maximum extinction at 328nm as seen from Figure 1
Degree, therefore the maximum absorption wavelength of chlorogenic acid is determined as 328nm, subsequent detection wavelength is set as 328nm.
The drafting of standard curve
Chlorogenic acid titer 0.00,2.00,4.00,8.00,12.00,16.00,20.00mL is taken to hold in 7 50mL respectively
In measuring bottle, add 70% ethyl alcohol constant volume, shake up, survey absorbance, draws standard curve, as a result as shown in Figure 2.It is obtained by Fig. 2 green
The equation of the standard curve of ortho acid is Y=0.0285X-0.011, R2=0.9989, linear relationship is good.
The extraction of sample Content of Chlorogenic Acid
Yellow fruit eggplant sample powder (Honghe Geju City county) 2g (being accurate to 0.01g) is weighed in 250mL round-bottomed flask, is added
160mL70% ethanol solution, is heated to reflux 1.5h, is cooled to room temperature and is filtered under diminished pressure, and records the volume of filtrate, takes its extracting solution
For 1.00mL in 50mL volumetric flask, 70% ethanol solution is settled to scale, shakes up, and surveys its absorbance, calculates recovery rate.
Recovery rate E (%)=(C × V)/M
In formula: the content (g/mL) of C expression filtrate Content of Chlorogenic Acid；The volume (mL) of V expression filtrate；M indicates yellow fruit eggplant powder
Last quality (g).
Influence and discussion of the single factor test to yellow fruit eggplant chlorogenic acid yield
Influence of the extractant to yellow fruit eggplant chlorogenic acid yield
Chlorogenic acid of the different extractants in other conditions under the same conditions refluxing extraction yellow fruit eggplant is chosen, according to filter
You can get it the optimum extraction agent of liquid absorbance size, experimental result are as shown in Figure 3.Different extractants is to green original as shown in Figure 3
The extraction effect of acid is different, the results showed that ethyl alcohol ﹥ distilled water ﹥ methanol ﹥ acetone, wherein the recovery rate of ethyl alcohol and distilled water differs not
Greatly, it is contemplated that the factors such as environmental protection, economic cost and practicability choose extractant of the distilled water as chlorogenic acid.
Influence of the liquid-to-solid ratio to yellow fruit eggplant chlorogenic acid yield
6 parts of yellow fruit eggplant sample 0.60g of precise in 150mL round-bottomed flask, respectively by liquid-to-solid ratio (mL/g) 20:1,
Distilled water is added in 30:1,40:1,50:1,60:1,70:1, under identical temperature, time conditions in refluxing extraction yellow fruit eggplant
Chlorogenic acid is cooled to room temperature, and is filtered under diminished pressure, and is recorded the volume of filtrate respectively, is taken its extracting solution 1.00mL in 50mL volumetric flask
Constant volume is diluted, its absorbance is surveyed, calculates chlorogenic acid yield.It is measured in parallel 3 times, experimental result is as shown in Figure 4.It can be with by Fig. 4
Before finding out that liquid-to-solid ratio is 40:1, recovery rate increases with the increase of liquid-to-solid ratio；When liquid-to-solid ratio reaches 40:1, chlorogenic acid is mentioned
Take rate maximum 0.196%；Be declined slightly later with the increase of liquid-to-solid ratio, it may be possible to because liquid-to-solid ratio increase be concentrated by evaporation and
The load being filtered under diminished pressure, causes recovery rate to be declined slightly.Therefore the best liquid-to-solid ratio that chlorogenic acid extracts is 40:1.
Influence of the temperature to yellow fruit eggplant chlorogenic acid yield
Distilled water is added in 150mL round-bottomed flask, by liquid-to-solid ratio 40:1 in 6 parts of yellow fruit eggplant sample 0.60g of precise, point
The refluxing extraction identical time not in the thermostat water bath at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, it is cooled to room
Temperature is filtered under diminished pressure, and is recorded the volume of filtrate respectively, is taken its extracting solution 1.00mL to dilute constant volume in 50mL volumetric flask, survey its suction
Luminosity calculates chlorogenic acid yield.It is measured in parallel 3 times, experimental result is as shown in Figure 5.As shown in Figure 5, before 80 DEG C, recovery rate
It increases and increases with temperature；When temperature is 80 DEG C, the recovery rate maximum 0.113% of chlorogenic acid；More than 80 DEG C recovery rates slightly under
Drop, this may be due to the catechol structural instability in chlorogenic acid molecular structure, and part chlorogenic acid can oxygen when the temperature is excessively high
Change and decompose, declines recovery rate.Therefore the optimum extraction temperature of chlorogenic acid is 80 DEG C.
Influence of the pH value to yellow fruit eggplant chlorogenic acid yield
6 parts of yellow fruit eggplant sample 0.60g of precise are in 150mL round-bottomed flask, by liquid-to-solid ratio 40:1, be added pH value be 2,
3,5,7,9,11 distilled water, the refluxing extraction same time in 80 DEG C of thermostat water bath, is cooled to room temperature, depressurized respectively
Filter records the volume of filtrate respectively, takes its extracting solution 1.00mL to dilute constant volume in 50mL volumetric flask, survey its absorbance, calculates
Chlorogenic acid yield.It is measured in parallel 3 times, experimental result is as shown in Figure 6.It will be appreciated from fig. 6 that as pH value < 3, the extraction of chlorogenic acid
Rate increases with pH value and is increased；When pH value=3, recovery rate maximum 0.102%；As pH value > 3, recovery rate increases with pH value
And reduce, it is polarity acid that this, which may be because of chlorogenic acid, it is more stable in acidic environment, with the increase of pH value, chlorogenic acid meeting
There is the phenomenon that dissolution, its recovery rate is caused to decline.Therefore the optimal pH of chlorogenic acid extractant is 3.
Influence of the time to yellow fruit eggplant chlorogenic acid yield
6 parts of yellow fruit eggplant sample 0.60g of precise are in 150mL round-bottomed flask, and by liquid-to-solid ratio 40:1, it is 3 that pH value, which is added,
Distilled water, refluxing extraction 0.5,1.0,1.5,2.0,2.5,3.0h in 80 DEG C of thermostat water bath, are cooled to room temperature respectively,
It is filtered under diminished pressure, records the volume of filtrate respectively, take its extracting solution 1.00mL to dilute constant volume in 50mL volumetric flask, survey its extinction
Degree calculates chlorogenic acid yield.It is measured in parallel 3 times, experimental result is as shown in Figure 7.As shown in Figure 7, upon extracting between t < 1.5h
When, the increase at any time of the recovery rate of chlorogenic acid and increase；Work as t=1.5h, the recovery rate maximum 0.098% of chlorogenic acid；As t >
When 1.5h, this may be due to the catechol structural instability in chlorogenic acid molecular structure, and prolonged heating can make green original
Acid oxidase decomposes, and recovery rate is caused to decline.Recovery rate increase at any time and decline, therefore optimum extraction time that chlorogenic acid extracts
For 1.5h.
Response surface optimization design result and discussion
Response surface optimization experimental method and result
On the basis of experiment of single factor, liquid-to-solid ratio, temperature, time, pH value=4 factor and level value are determined, use
10.0 software of Design-Expert carries out the design of Box-Behnken response surface and data analysis.The high, normal, basic water of each factor
Divide equally and do not encoded with 1,0, -1, each experimental factor and level value are shown in Table 1.
1 experimental factor of table and level
Using Box-Behnken center combination experimental design principle, in conjunction with single factor experiment as a result, liquid-to-solid ratio 40:1, temperature
Spend 80 DEG C, time 1.5h, pH value 4.Experimental design and the results are shown in Table 2.
The design of 2 response surface experiments of table and result
Multiple regression fitting is carried out to data in table 2 using 8.0 Trial software of Design-Expert, obtains table 3.
3 regression model of table and its significance test
Last regression line equation is simulated by software are as follows:
Y=-2.38904+0.022925A+0.041658B+0.329C+0.14917D+0.000028A B+0.0029AC-
0.0002AD-0.0021BC-0.000125BD-0.0125AC-0.00034A2-0.00024B2-0.089C2-0.02D2, in which:
A indicates liquid-to-solid ratio；B indicates temperature；C indicates the time；D indicates pH value.
By the results of analysis of variance it is found that the regression equation is in extremely significant property (P < 0.01), it is also in extremely significant that model, which loses quasi- item,
Property (P < 0.01).A,C,A2、B2、C2、D2Influence to chlorogenic acid yield is extremely significant (P < 0.01)；B,D,AB,AC,AD,
The influence of BC, BD to chlorogenic acid yield is not significant (P > 0.05).
By the simulation of regression equation, influence of the mutual response to chlorogenic acid yield two-by-two between four single factor tests is obtained
To corresponding response surface result as shown in Fig. 8~18:
Fig. 8 is the influence contour map of temperature and liquid-to-solid ratio to recovery rate, and Fig. 9 is the shadow of temperature and liquid-to-solid ratio to recovery rate
Figure is rung, Figure 10 is the influence contour map of temperature and pH value to recovery rate, and Figure 11 is the influence of temperature and pH value to recovery rate, figure
12 be influence contour map of the temperature and time to recovery rate, and Figure 13 is influence of the temperature and time to recovery rate, and Figure 14 is liquid
Material ratio and influence contour map of the pH value to recovery rate, Figure 15 are the influence of liquid-to-solid ratio and pH value to recovery rate, and Figure 16 is liquid material
Than the influence contour map with the time to recovery rate, Figure 17 is the influence of liquid-to-solid ratio and time to recovery rate, Figure 18 be pH value and
Influence contour map of the time to recovery rate, Figure 19 are the influence of pH value and time to recovery rate.
Recovery rate first increases and reduces afterwards with the variation of temperature in Fig. 9, and the variation tendency of liquid-to-solid ratio is similar.90 DEG C of temperature,
When liquid-to-solid ratio 50:1, recovery rate reaches maximum.The variation curved surface of temperature is steeper, by 8 contour map it can also be seen that temperature
Direction contour is intensive, illustrates that influence of the temperature to recovery rate is greater than influence of the liquid-to-solid ratio to recovery rate.
Recovery rate variation with temperature in Figure 11, first increases and reduces afterwards, and the variation tendency of pH value is similar, and 80 DEG C of temperature, pH
Value=3, recovery rate are maximum.The variation curved surface of pH value is steeper, by 10 contour map it can also be seen that pH value direction contour
Intensively, illustrate that influence of the pH value to recovery rate is greater than influence of the temperature to recovery rate.
Recovery rate first increases and reduces afterwards with the variation of time in Figure 13, and the variation tendency of temperature is similar, and 80 DEG C of temperature,
Time 1.5h, recovery rate are maximum.In contrast, the variation curved surface of time is steeper than the variation curved surface of temperature, by 12 contour map
It can also be seen that time orientation contour is intensive, illustrate that influence of the time to recovery rate is greater than influence of the temperature to recovery rate.
Recovery rate first increases and reduces afterwards with the variation of pH value in Figure 15, and the variation tendency of liquid-to-solid ratio is similar, pH value=4,
Liquid-to-solid ratio 50:1, recovery rate are maximum.The variation curved surface of pH value is steeper, the pH value direction it can be seen from 14 contour map
Contour is intensive, illustrates that influence of the pH value to recovery rate is greater than influence of the liquid-to-solid ratio to recovery rate.
Recovery rate first increases and reduces afterwards with the variation of time in Figure 17, and the variation tendency of liquid-to-solid ratio is similar, time 2h,
Liquid-to-solid ratio 50:1, recovery rate reach maximum.In contrast, the variation curved surface of time is steeper than the variation curved surface of liquid-to-solid ratio, by 16
The contour that contour map can be seen that time orientation is intensive, illustrates that influence of the time to recovery rate is greater than liquid-to-solid ratio to extraction
The influence of rate.
Recovery rate first increases and reduces afterwards with the variation of pH value in Figure 19, and the variation tendency of time is similar, pH value=3, when
Between 1.5h, recovery rate reaches maximum.The variation curved surface of time is steep compared to the variation curved surface of pH value, can be with by 18 contour map
Find out, the contour of time orientation is intensive, illustrates that influence of the time to recovery rate is greater than influence of the pH value to recovery rate.
Result verification and discussion
By response surface optimization as a result, Binding experiment room actual conditions obtain the optimum extraction scheme of yellow fruit eggplant Content of Chlorogenic Acid
Be: using distilled water as extractant, liquid-to-solid ratio 50mL:1g, temperature is 90 DEG C, pH value 2, time 1h, and chlorogenic acid mentions
Take rate maximum 0.28%.In selected each factor range, according to the influence sequence of response, 4 factors mention chlorogenic acid
Taking the influence sequence of rate is: time > pH value > temperature > liquid-to-solid ratio.
Different regions yellow fruit eggplant Content of Chlorogenic Acid compares
The optimum extraction scheme that face obtains according to response has carried out comparision contents to different regions yellow fruit eggplant Content of Chlorogenic Acid,
The results are shown in Table 4.As can be seen from Table 4, a certain amount of chlorogenic acid is contained in yellow fruit eggplant；The content of different regions chlorogenic acid
Different, the yellow fruit eggplant Content of Chlorogenic Acid highest of Puer City Simao District, the yellow fruit eggplant Content of Chlorogenic Acid of Qujing Shizong County contains
Measure minimum, but gap is little, it may be possible to because the influence of topography and weather, the content of yellow fruit eggplant Content of Chlorogenic Acid have differences.
The content of 4 different regions yellow fruit eggplant Content of Chlorogenic Acid of table
The present invention uses Star point design-response surface optimization method design experiment, is from change with liquid-to-solid ratio, temperature, time, pH value
Amount, recovery rate is dependent variable, utilizes equation of linear regression and binomial fitting, the optimum extraction process of yellow fruit eggplant Content of Chlorogenic Acid
Be: distilled water is as extractant, and liquid-to-solid ratio 50mL:1g, 90 DEG C of temperature, the recovery rate of pH value 2, time 1h, chlorogenic acid is maximum
0.28%, it is close with prediction 0.268%.Wherein 4 process conditions to the influence degree of chlorogenic acid yield from big to small are as follows: when
Between > pH value > temperature > liquid-to-solid ratio.
The above is only a preferred embodiment of the present invention, it is not intended to limit the present invention in any form.It should
It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (10)
1. a kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid, which comprises the following steps:
Refluxing extraction is carried out after yellow fruit eggplant sample powder is mixed with water, the pH value of the water is 2~11.
2. extracting method according to claim 1, which is characterized in that the pH value of the water is 2~3.
3. extracting method of any of claims 1 or 2, which is characterized in that the water and the liquid-to-solid ratio of yellow fruit eggplant sample powder are
20~70mL:1g.
4. extracting method according to claim 1, which is characterized in that the temperature of the refluxing extraction is 40~90 DEG C.
5. extracting method according to claim 1 or 4, which is characterized in that the time of the refluxing extraction is 0.5~3h.
6. extracting method according to claim 5, which is characterized in that the time of the refluxing extraction is 1.5~2h.
7. extracting method according to claim 1, which is characterized in that the temperature of the refluxing extraction is 90 DEG C, and the time is
The liquid-to-solid ratio of 1h, water and yellow fruit eggplant sample powder is 50mL:1g, and the pH value of water is 2.
8. extracting method according to claim 1, which is characterized in that the temperature of the refluxing extraction is 80 DEG C, and the time is
The liquid-to-solid ratio of 1.5h, water and yellow fruit eggplant sample powder is 40mL:1g, and the pH value of water is 4.
9. extracting method according to claim 1, which is characterized in that the yellow fruit eggplant sample powder sieves with 100 mesh sieve.
10. extracting method according to claim 1, which is characterized in that the place of production of the yellow fruit eggplant sample powder includes general
Pu'er tea Simao, Red River Geju City, Qujing Luoping, Qujing master of great learning and integrity, Chuxiong Wuding County, Pu'er Jing Dong, Kunming Xun Dian or mountain of papers Maguan.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910541341.2A CN110156604A (en) | 2019-06-21 | 2019-06-21 | A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910541341.2A CN110156604A (en) | 2019-06-21 | 2019-06-21 | A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110156604A true CN110156604A (en) | 2019-08-23 |
Family
ID=67626375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910541341.2A Pending CN110156604A (en) | 2019-06-21 | 2019-06-21 | A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110156604A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302156A (en) * | 2007-05-08 | 2008-11-12 | 中国农业科学院植物保护研究所 | Process for extracting chlorogenic acid from Eupatorium adenophorum |
| CN101337001A (en) * | 2008-02-15 | 2009-01-07 | 上海海天医药科技开发有限公司 | Solanum xanthocarpum extract, preparation method and use thereof |
| JP2015051932A (en) * | 2013-09-05 | 2015-03-19 | 富士フイルム株式会社 | Manufacturing method of chlorogenic acid |
| CN104974041A (en) * | 2014-04-12 | 2015-10-14 | 兰赫(上海)生物科技有限公司 | High-purity chlorogenic acid, preparation method and application thereof |
| CN109456188A (en) * | 2018-12-12 | 2019-03-12 | 黑龙江东方学院 | A kind of combined extraction separation purification process of Chlorogenic Acid of Flos Lonicerae and general flavone |
-
2019
- 2019-06-21 CN CN201910541341.2A patent/CN110156604A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302156A (en) * | 2007-05-08 | 2008-11-12 | 中国农业科学院植物保护研究所 | Process for extracting chlorogenic acid from Eupatorium adenophorum |
| CN101337001A (en) * | 2008-02-15 | 2009-01-07 | 上海海天医药科技开发有限公司 | Solanum xanthocarpum extract, preparation method and use thereof |
| JP2015051932A (en) * | 2013-09-05 | 2015-03-19 | 富士フイルム株式会社 | Manufacturing method of chlorogenic acid |
| CN104974041A (en) * | 2014-04-12 | 2015-10-14 | 兰赫(上海)生物科技有限公司 | High-purity chlorogenic acid, preparation method and application thereof |
| CN109456188A (en) * | 2018-12-12 | 2019-03-12 | 黑龙江东方学院 | A kind of combined extraction separation purification process of Chlorogenic Acid of Flos Lonicerae and general flavone |
Non-Patent Citations (3)
| Title |
|---|
| KOMAL M. PARMAR ET AL.: "Wound healing potential of Solanum xanthocarpum in streptozotocin-induced diabetic rats", 《JOURNAL OF PHARMACY AND PHARMACOLOGY》 * |
| 潘雪峰等: "山银花叶中绿原酸水提工艺研究", 《中国农学通报》 * |
| 王茜等: "杜仲叶中绿原酸提取分离工艺条件的研究", 《离子交换与吸附》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105717229B (en) | A kind of method for determining 11 kinds of flavones ingredients in vine tea simultaneously with HPLC | |
| Gogou et al. | Particulate-dissolved transformations as a sink for semi-labile dissolved organic matter: Chemical characterization of high molecular weight dissolved and surface-active organic matter in seawater and in diatom cultures | |
| CN106872233A (en) | A kind of 5 hydroxymethylfurfural cysteine adducts and preparation method and application and detection method | |
| CN104922196A (en) | General ohwia flavone extract preparation method and general ohwia flavone extract quality detecting method | |
| CN101921494B (en) | Preparation method of red pigment from camellia japonica | |
| CN105560888B (en) | A kind of method of polyphenol component leaching rate in raising dendrobium candidum | |
| CN103869019B (en) | The method for building up of the HPLC finger-print of a kind of Fenggang zinc selenium tea | |
| CN102743598B (en) | var. Denneanum extract and formula particles thereof | |
| CN110156604A (en) | A kind of extracting method of yellow fruit eggplant Content of Chlorogenic Acid | |
| CN103830306A (en) | Preparation method of honey suckle leaf effective extract product | |
| CN104644815A (en) | Method for extracting total flavonoids of Chinese wampee leaves employing two-phase aqueous system and ultrasonic integration | |
| Khan et al. | Analysis of major polyphenolic compounds of Cydonia oblonga Miller (Quince) fruit extract by UPLC-MS/MS and its effect on adipogenesis in 3T3-L1 cells | |
| CN104530147B (en) | A kind of extraction from callicarpa nudiflora leaf prepares the method for verbascoside standard substance | |
| Pilić et al. | The anti-corrosion behaviour of Satureja montana L. extract on iron in NaCl solution | |
| CN103908513B (en) | The extracting method of shinyleaf yellowhorn fruit shell total saponins | |
| CN109828053A (en) | The raw HERBA DENDROBII of a kind of pair of stone and the method for setting raw HERBA DENDROBII progress chromatographic identification | |
| CN109453272A (en) | A kind of preparation method of sea calamus high anti-oxidation activity extract | |
| Wang et al. | DES Based Efficient Extraction Method for Bioactive Coumarins from Angelica dahurica (Hoffm.) Benth. & Hook. f. ex Franch. & Sav. | |
| Han et al. | Characteristics of stable hydrogen and oxygen isotopes of soil moisture under different land use in dry hot valley of Yuanmou | |
| CN104535513A (en) | Glabrous sarcandra herb extract and detection method of preparation thereof | |
| CN109100463A (en) | The extraction purification and the method for inspection of astragalin in a kind of BEIQI MUSHROOM | |
| CN109053756A (en) | Phenylpropanoid Glycosides class ester catechin and its preparation method and application | |
| CN105153320B (en) | The extracting method of one Polysaccharides From Laminaria Japonica | |
| CN108218935B (en) | Method for extracting myricitrin, quercitrin and afzelin from Chinese redbud leaves by using ionic liquid | |
| CN105596257A (en) | Xanthoceras leaf antioxidant active material, extraction method and application in cosmetics |
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 |
Application publication date: 20190823 |
|
| RJ01 | Rejection of invention patent application after publication |