CN108658770A - A method of preparing chlorogenic acid monomer from Black King Kong potato - Google Patents
A method of preparing chlorogenic acid monomer from Black King Kong potato Download PDFInfo
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- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- 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
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The invention discloses a kind of methods that chlorogenic acid monomer is prepared in potato from Black King Kong, include the following steps:(1) extracting solution is added into Black King Kong potato powder and prepares chlorogenic acid extracting solution;(2) the chlorogenic acid extracting solution is passed through into macroporous resin adsorption column with the flow velocity of 1~3mL/min, is washed with water and after ethanol elution, obtains chlorogenic acid crude product;(3) chlorogenic acid crude product is configured to the first solution of chlorogenic acid, and the first solution of chlorogenic acid is extracted with ethyl acetate 1~2 time, collect ethyl acetate layer, concentrated dry chlorogenic acid fine work;(4) chlorogenic acid fine work is configured to the second solution of chlorogenic acid, is detached with the second solution of chlorogenic acid of semi-preparative liquid chromatogram pair, the sample of collection is concentrated with after drying, obtain chlorogenic acid monomer.The present invention reaches 97~99% by solvent extraction method, ethyl acetate extraction and half preparative high-performance liquid chromatographic chlorogenic acid extracting from Black King Kong potato, the purity of chlorogenic acid monomer obtained.
Description
Technical field
The invention belongs to chlorogenic acid monomer preparing technical fields, and in particular to one kind preparing green original from Black King Kong potato
The method of acid monomers.
Background technology
Chlorogenic acid is a kind of organic acid containing hydroxyl and adjacent two phenolic hydroxyl groups, the entitled 5-O- coffee acyls chinic acid of chemistry,
It is a kind of phenylpropanoids that plant generates during aerobic respiration through shikimic acid pathway.Chlorogenic acid is a kind of important
Bioactive substance, have extensive pharmacological action and bioactivity, be not only numerous medicinal materials and Chinese patent drug antibacterial and detoxicating, disappear
The principle active component of scorching cholagogic, also have it is antiviral, increase white blood cell, be antitumor, lowering blood pressure and blood fat, remove free radical
The effects that with stimulating central nervous system system.Chlorogenic acid is widely present in plant, higher with the content in honeysuckle, Cortex Eucommiae, mesh
The preceding mainly chlorogenic acid extracting from the plants such as honeysuckle and Cortex Eucommiae.
The kind skin of Black King Kong potato is pitch-black shinny and rich in gloss, darkly purple due to it is rich in purple anthocyanidin, it
It is China's introducing and planting, integrates the rare Potato Cultivars of medicine-food two-purpose.At present both at home and abroad in Black King Kong potato
The research of active constituent focuses primarily upon natural pigment, but this seminar is contained in Fan County Black King Kong potato in the course of the research
A kind of substance more more rich than pigment content, after carrying out monomer separation, purifying and structural characterization to the substance, it was demonstrated that the object
Matter is chlorogenic acid.The current mainly chlorogenic acid extracting from the plants such as honeysuckle and Cortex Eucommiae, such as:Number of patent application is
201710075147.0 application documents disclose a kind of method of the chlorogenic acid extracting from green coffee bean, mainly utilize equipment
It extracts;The application documents that number of patent application is 201711344050.1 disclose a kind of side of the chlorogenic acid extracting from Cortex Eucommiae
Method is mainly extracted by enzyme solution;The application documents that number of patent application is 201810154455.7 disclose a kind of from new
The method of chlorogenic acid extracting in fresh sweet potato leaves uses ultrasonic extraction, microwave radiation technology second to ensure extraction efficiency
Assisted Ethanol extraction method is followed the example of and is digested in alcohol extracting.There is not yet from Black King Kong potato chlorogenic acid extracting report, and first
It needs to use spray drying unit in item invention, the requirement to equipment is high, and the purity of chlorogenic acid extracting is relatively low, only
70.3%, the functional study as plasmid standards for quantitation and chlorogenic acid cannot be met;The side using enzymolysis is needed in two inventions afterwards
Method introduces enzyme and enzymolysis product during enzymolysis, increases the difficulty isolated and purified, and extract the pure of obtained chlorogenic acid
Degree is still not high enough.
Invention content
It is an object of the invention to overcome above-mentioned technical deficiency, a kind of extracting method that chlorogenic acid monomer purity is high is proposed,
Another object of the present invention is to provide a kind of methods of chlorogenic acid extracting in potato from Black King Kong.
To reach above-mentioned technical purpose, technical scheme of the present invention provides one kind and preparing chlorogenic acid from Black King Kong potato
The method of monomer, includes the following steps:
S1. extracting solution is added into Black King Kong potato powder and prepares chlorogenic acid extracting solution;
S2. the chlorogenic acid extracting solution is passed through into macroporous resin adsorption column with the flow velocity of 1~3mL/min, after adsorption saturation,
Macroporous resin adsorption column is washed with water, then chlorogenic acid is eluted with ethanol solution, collects eluent, it is concentrated dry that chlorogenic acid is thick
Product;
S3. the chlorogenic acid crude product is configured to the first solution of chlorogenic acid, and the described first green original is extracted with ethyl acetate
Acid solution 1~2 time collects ethyl acetate layer, concentrated dry chlorogenic acid fine work;
S4. the chlorogenic acid fine work is configured to the second solution of chlorogenic acid, with semi-preparative liquid chromatogram to described second
Solution of chlorogenic acid is detached, and with formic acid solution-acetonihile gradient elution, collects the sample of 13.3~14.3min of retention time, then
After concentrated and dry, chlorogenic acid monomer is obtained.
Compared with prior art, beneficial effects of the present invention include:
1, the present invention is extracted by solvent extraction method, one step of ethyl acetate, and the purity of extract liquor Content of Chlorogenic Acid reaches 72~
75%, then combine semi-preparative liquid chromatogram chlorogenic acid extracting monomer from Black King Kong potato, final chlorogenic acid list obtained
The purity of body reaches 97~99%, hence it is evident that produced by the present invention green higher than the purity for the chlorogenic acid monomer extracted in the prior art
The purity of ortho acid monomer reaches the requirement of plasmid standards for quantitation and functional study;
2, the chlorogenic acid monomer in the present invention is extracted from the anthocyanin extracting solution of Black King Kong potato with ethyl acetate
It obtains, to prepare the waste liquid part of anthocyanin, the waste of resource is avoided with waste liquid extracting section chlorogenic acid, is realized black
The comprehensive utilization of Buddha's warrior attendant potato;
3, China is just promoting potato as staple food grain product industrialization plan, and from the Chinese medicine materials such as honeysuckle and Cortex Eucommiae
Chlorogenic acid extracting is compared, and raw material sources are wide, resourceful, and the chlorogenic acid extracted will not remain the smell of Chinese herbal medicine;
4, extracting method of the invention is simple, and technological process is easily manipulated, and is suitble to industrial automatic control production.
Description of the drawings
Fig. 1 is the process flow chart of the chlorogenic acid extracting monomer from Black King Kong potato;
Fig. 2 is the efficient liquid phase chromatographic analysis figure of Black King Kong potato extract chlorogenic acid;
Fig. 3 be Black King Kong potato extract chlorogenic acid hydrogen spectrum (1HNMR) figure;
Fig. 4 be Black King Kong potato extract chlorogenic acid carbon spectrum (13CNMR) figure;
Fig. 5 is the DEPT135 spectrograms of Black King Kong potato extract chlorogenic acid.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The method that chlorogenic acid monomer is prepared in the potato provided by the invention from Black King Kong is further elaborated.Following embodiments
In experimental method be unless otherwise specified conventional method.It should be appreciated that specific embodiment described herein is only used
To explain the present invention, it is not intended to limit the present invention.
Embodiment 1:
The embodiment of the present invention 1 provides a kind of method that chlorogenic acid monomer is prepared in the potato from Black King Kong, including such as
Lower step:
(1) it extracts:It takes and cleans peeling without rotten Black King Kong potato, then potato is cut into inch strips, potato slices are existed
It dries at 50 DEG C, is crushed after drying, cross 40 mesh sieve, obtain Black King Kong potato powder;By 2g Black King Kong potato powder
It is added in a concentration of 0.3mol/L hydrochloric acid solutions of 120mL, after then extracting 2h at 70 DEG C, leaching liquor is transferred in centrifuge,
Under conditions of rotating speed is 8000r/min, 10min is centrifuged, obtained supernatant is chlorogenic acid extracting solution;
(2) crude chlorogenic acid powder is made:The chlorogenic acid extracting solution obtained in step (1) is passed through with the flow velocity of 1mL/min
The adsorption column filled with macroreticular resin D101 types is crossed to be washed greatly with the flow velocity of 1mL/min with deionized water after Dynamic Adsorption is saturated
Hole resin absorbing column is colourless to efflux, then big with the flow velocity elution of 1mL/min with the ethanol solution that volume fraction is 60%
The chlorogenic acid of hole resin adsorption, collection ethanol eluate is flowed out up to no chlorogenic acid, then subtracts the eluent of collection at 50 DEG C
Pressure is concentrated into paste, obtains chlorogenic acid concentrate, chlorogenic acid concentrate is freeze-dried to obtain crude chlorogenic acid powder 14.2mg;
(3) the refined chlorogenic acid powder of system:Suitable deionized water is added into crude chlorogenic acid powder, makes crude
Chlorogenic acid powder is completely dissolved, and obtains the first solution of chlorogenic acid, and the acetic acid of 2 times of volumes is then added into the first solution of chlorogenic acid
Ethyl ester extracts 1 time, collects ethyl acetate layer and is concentrated and dried, obtains refined chlorogenic acid powder 5.7mg, purity 72%;
(4) it isolates and purifies:According to volume ratio it is 1 by 0.3% formic acid and acetonitrile:9 are made into solvent, to refined chlorogenic acid
Suitable solvent is added in powder, chlorogenic acid powder is made to be completely dissolved, obtains the second solution of chlorogenic acid, with semi-preparative liquid chromatogram
The second solution of chlorogenic acid of instrument pair isolates and purifies, and the condition isolated and purified is:Chromatographic column is Daisogel C18Column (20mm ×
250mm, 10 μm), Detection wavelength 324nm, the formic acid (A) and acetonitrile (B) that mobile phase is 0.3%, gradient elution program is as follows:
When 0min, mobile phase A 80%, Mobile phase B 20%;
When 5min, mobile phase A 80%, Mobile phase B 20%;
When 13min, mobile phase A 70%, Mobile phase B 30%;
When 17min, mobile phase A 65%, Mobile phase B 35%;
When 20min, mobile phase A 65%, Mobile phase B 35%;
When 21min, mobile phase A 70%, Mobile phase B 30%;
When 30min, mobile phase A 80%, Mobile phase B 20%.
Flow velocity is 15mL/min, sample size 2mL, collects the sample of retention time 13.3-14.3min, by being concentrated under reduced pressure
After removing solvent and freeze-drying, chlorogenic acid monomer 3.3mg, purity 97% are obtained.
Embodiment 2:
The embodiment of the present invention 2 provides a kind of method that chlorogenic acid monomer is prepared in the potato from Black King Kong, including such as
Lower step:
(1) it extracts:It takes and cleans peeling without rotten Black King Kong potato, then potato is cut into inch strips, potato slices are existed
It dries at 50 DEG C, is crushed after drying, cross 40 mesh sieve, obtain Black King Kong potato powder;By 2g Black King Kong potato powder
It is added in a concentration of 0.1mol/L hydrochloric acid solutions of 160mL, after then extracting 1h at 70 DEG C, leaching liquor is transferred to centrifugal separator
In, under conditions of rotating speed is 8000r/min, 10min is centrifuged, obtained supernatant is chlorogenic acid extracting solution;
(2) crude chlorogenic acid powder is made:The chlorogenic acid extracting solution obtained in step (1) is passed through with the flow velocity of 1mL/min
The adsorption column filled with macroreticular resin AB-8 types is crossed to be washed greatly with the flow velocity of 3mL/min with deionized water after Dynamic Adsorption is saturated
Hole resin absorbing column is colourless to efflux, then big with the flow velocity elution of 1mL/min with the ethanol solution that volume fraction is 60%
The chlorogenic acid of hole resin adsorption, collection ethanol eluate is flowed out up to no chlorogenic acid, then subtracts the eluent of collection at 50 DEG C
Pressure is concentrated into paste, obtains chlorogenic acid concentrate, chlorogenic acid concentrate is freeze-dried to obtain crude chlorogenic acid powder 12.8mg;
(3) the refined chlorogenic acid powder of system:Suitable deionized water is added into crude chlorogenic acid powder, makes crude
Chlorogenic acid powder is completely dissolved, and obtains the first solution of chlorogenic acid, and the acetic acid of 2 times of volumes is then added into the first solution of chlorogenic acid
Ethyl ester extracts 2 times, and collection, combined ethyl acetate layer are simultaneously concentrated and dried, and obtain refined chlorogenic acid powder 5.1mg, purity is
73%;
(4) it isolates and purifies:According to volume ratio it is 1 by 0.3% formic acid and acetonitrile:9 are made into solvent, to refined chlorogenic acid
Suitable solvent is added in powder, chlorogenic acid powder is made to be completely dissolved, obtains the second solution of chlorogenic acid, with semi-preparative liquid chromatogram
The second solution of chlorogenic acid of instrument pair isolates and purifies, and is isolated and purified using purification condition same as Example 1, receives
The monomer peak for collecting retention time 13.3-14.3min obtains chlorogenic acid list after being concentrated under reduced pressure and removing solvent and freeze-drying
Body 2.96mg, purity 98%.
Embodiment 3:
The embodiment of the present invention 3 provides a kind of method that chlorogenic acid monomer is prepared in the potato from Black King Kong, including such as
Lower step:
(1) it extracts:It takes and cleans peeling without rotten Black King Kong potato, then potato is cut into inch strips, potato slices are existed
It dries at 40 DEG C, is crushed after drying, cross 80 mesh sieve, obtain Black King Kong potato powder;By 20g Black King Kong potato powder
It is added in a concentration of 2wt% citric acid solutions of 1200mL, after then extracting 2h at 60 DEG C, leaching liquor is transferred to centrifugal separator
In, under conditions of rotating speed is 6000r/min, 10min is centrifuged, obtained supernatant is chlorogenic acid extracting solution;
(2) crude chlorogenic acid powder is made:The chlorogenic acid extracting solution obtained in step (1) is passed through with the flow velocity of 1mL/min
The adsorption column filled with macroreticular resin X-5 types is crossed to be washed greatly with the flow velocity of 3mL/min with deionized water after Dynamic Adsorption is saturated
Hole resin absorbing column is colourless to efflux, then big with the flow velocity elution of 3mL/min with the ethanol solution that volume fraction is 80%
The chlorogenic acid of hole resin adsorption, collection ethanol eluate is flowed out up to no chlorogenic acid, then subtracts the eluent of collection at 50 DEG C
Pressure is concentrated into paste, obtains chlorogenic acid concentrate, chlorogenic acid concentrate is freeze-dried to obtain crude chlorogenic acid powder
136.2mg;
(3) the refined chlorogenic acid powder of system:Suitable deionized water is added into crude chlorogenic acid powder, makes crude
Chlorogenic acid powder is completely dissolved, and obtains the first solution of chlorogenic acid, and the acetic acid of 1 times of volume is then added into the first solution of chlorogenic acid
Ethyl ester extracts 1 time, collects ethyl acetate layer and is concentrated and dried, obtains refined chlorogenic acid powder 54.8mg, purity 74%;
(4) it isolates and purifies:According to volume ratio it is 1 by 0.3% formic acid and acetonitrile:9 are made into solvent, to refined chlorogenic acid
Suitable solvent is added in powder, chlorogenic acid powder is made to be completely dissolved, obtains the second solution of chlorogenic acid, with semi-preparative liquid chromatogram
The second solution of chlorogenic acid of instrument pair isolates and purifies, and is isolated and purified using purification condition same as Example 1, receives
The monomer peak for collecting retention time 13.3-14.3min obtains chlorogenic acid list after being concentrated under reduced pressure and removing solvent and freeze-drying
Body 31.5mg, purity 98%.
Embodiment 4:
The embodiment of the present invention 4 provides a kind of method that chlorogenic acid monomer is prepared in the potato from Black King Kong, including such as
Lower step:
(1) it extracts:It takes and cleans peeling without rotten Black King Kong potato, then potato is cut into inch strips, potato slices are existed
It dries at 50 DEG C, is crushed after drying, cross 40 mesh sieve, obtain Black King Kong potato powder;By 20g Black King Kong potato powder
It is added in a concentration of 4wt% citric acid solutions of 1600mL, after then extracting 2h at 50 DEG C, leaching liquor is transferred to centrifugal separator
In, under conditions of rotating speed is 4000r/min, 15min is centrifuged, obtained supernatant is chlorogenic acid extracting solution;
(2) crude chlorogenic acid powder is made:The chlorogenic acid extracting solution obtained in step (1) is passed through with the flow velocity of 3mL/min
The adsorption column filled with macroreticular resin DM130 types is crossed to be washed with the flow velocity of 3mL/min with deionized water after Dynamic Adsorption is saturated
Macroporous resin adsorption column is colourless to efflux, then elutes quilt with the ethanol solution that volume fraction is 80% with the flow velocity of 3mL/min
The chlorogenic acid of macroporous resin adsorption, collection ethanol eluate are flowed out up to no chlorogenic acid, then by the eluent of collection at 50 DEG C
It is concentrated under reduced pressure into paste, obtains chlorogenic acid concentrate, chlorogenic acid concentrate is freeze-dried to obtain crude chlorogenic acid powder
136.7mg;
(3) the refined chlorogenic acid powder of system:Suitable deionized water is added into crude chlorogenic acid powder, makes crude
Chlorogenic acid powder is completely dissolved, and obtains the first solution of chlorogenic acid, and the acetic acid of 1 times of volume is then added into the first solution of chlorogenic acid
Ethyl ester extracts 1 time, collects ethyl acetate layer and is concentrated and dried, obtains refined chlorogenic acid powder 54.9mg, purity 75%;
(4) it isolates and purifies:According to volume ratio it is 1 by 0.3% formic acid and acetonitrile:9 are made into solvent, to refined chlorogenic acid
Suitable solvent is added in powder, chlorogenic acid powder is made to be completely dissolved, obtains the second solution of chlorogenic acid, with semi-preparative liquid chromatogram
The second solution of chlorogenic acid of instrument pair isolates and purifies, and is isolated and purified using purification condition same as Example 1, receives
The monomer peak for collecting retention time 13.3-14.3min obtains chlorogenic acid list after being concentrated under reduced pressure and removing solvent and freeze-drying
Body 37.1mg, purity 99%.
The chlorogenic acid monomer extracted in the embodiment of the present invention 1~4 is analyzed and identified with the following method:
(1) purity of analytic type liquid-phase chromatographic analysis chlorogenic acid monomer, detaches with the following method:Chromatographic column is
DaisogelC18Column (20mm × 250mm, 10 μm), Detection wavelength 324nm, the formic acid (A) and acetonitrile that mobile phase is 0.3%
(B), gradient elution program is as follows:
When 0min, mobile phase A 90%, Mobile phase B 10%;
When 5min, mobile phase A 88%, Mobile phase B 12%;
When 13min, mobile phase A 79%, Mobile phase B 21%;
When 14min, mobile phase A 90%, Mobile phase B 10%;
When 16min, mobile phase A 90%, Mobile phase B 10%;
Flow velocity is 1mL/min, and 10 μ L of sample size, sample volume ratio is 1:9 0.3% formic acid and acetonitrile dissolving, point
Analysis result is shown in Fig. 2.
(2) chlorogenic acid monomer is identified:It is interior with tetramethylsilane (TMS) after four deuterated methanols (CD3OD) sample dissolution
Object is marked, sample is molten in Bruker 400MHZ (400 types of Avance III HD, Bruker companies of Switzerland) Nuclear Magnetic Resonance
Hydrogen spectrum (1HNMR), carbon spectrum (13CNMR) and the DEPT135 of liquid are composed, and measurement result is shown in Fig. 3~5.
As seen from Figure 2, the retention time at chlorogenic acid monomer peak is 5.358min, and the purity of chlorogenic acid monomer is 97
~99%.
By Fig. 3~5 it can be seen that under nuclear magnetic resonance measuring result:
1H-NMR(CD3OD):δ 7.55 (1H, d, J=15.8Hz, H-7 '), 7.04 (1H, br.S, H-2 '), 6.94 (1H,
Br.D, J=8.1Hz, H-6 '), 6.77 (1H, d, J=8.1Hz, H-5 '), 6.25 (1H, d, J=15.8Hz, H-8 '), 5.33
(1H, br.Dd, J=10.2,8.0Hz, H-5), 4.17 (1H, br.S, H-3), 3.72 (1H, br.D, J=8.0Hz, H-4),
1.98-2.28 (4H, m, H-2and H-6);
13C-NMR(CD3OD):δ 177.3 (s, C-7), 168.7 (s, C-9 '), 149.5 (s, C-4 '), 147.1 (d, C-
7 '), 146.8 (s, C-3 '), 127.8 (s, C-1 '), 123.0 (d, C-6 '), 116.5 (d, C-5 '), 115.3 (d, C-2 '),
115.2 (d, C-8 '), 76.3 (s, C-1), 73.6 (d, C-4), 72.0 (d, C-5), 71.4 (d, C-3), 38.9 (t, C-6),
38.2 (t, C-2).
Nuclear magnetic resonance measuring result and document【Yang Fengying, Su Yanfang, Wang Huaisong wait the chemical constitution study of Rhizoma Polygoni suffultis
[J] Chinese herbal medicines, 41 (8):1236-1239.】With【Saracoglu I,Harput U S,Calis I,et al.Phenolic
constituentsfromphlomis lycia[J].Turkish Journal ofChemistry,2002,26(1):133-
142.】As a result consistent, i.e., the substance that the present invention extracts is 5-O- coffee acyl chinic acids, i.e. chlorogenic acid.
The specific implementation mode of present invention described above, is not intended to limit the scope of the present invention..Any basis
The various other corresponding changes and deformation that the technical concept of the present invention is made, should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (10)
1. a kind of method for preparing chlorogenic acid monomer in potato from Black King Kong, which is characterized in that include the following steps:
S1. extracting solution is added into Black King Kong potato powder and prepares chlorogenic acid extracting solution;
S2. the chlorogenic acid extracting solution is passed through into macroporous resin adsorption column with the flow velocity of 1~3mL/min, after adsorption saturation, uses water
Macroporous resin adsorption column is washed, then chlorogenic acid is eluted with ethanol solution, collects eluent, concentrated dry chlorogenic acid crude product;
S3. the chlorogenic acid crude product is configured to the first solution of chlorogenic acid, and it is molten that first chlorogenic acid is extracted with ethyl acetate
Liquid 1~2 time collects ethyl acetate layer, concentrated dry chlorogenic acid fine work;
S4. the chlorogenic acid fine work is configured to the second solution of chlorogenic acid, with semi-preparative liquid chromatogram to the described second green original
Acid solution is detached, and with formic acid solution-acetonihile gradient elution, collects the sample of 13.3~14.3min of retention time, then through dense
After contracting and drying, chlorogenic acid monomer is obtained.
2. the method for preparing chlorogenic acid monomer in the potato according to claim 1 from Black King Kong, which is characterized in that step
Semi-preparative liquid chromatogram separation condition is in S4:Daisogel C18Chromatographic column, Φ 20 × 250mm, 10 μm;Flow velocity is 15mL/
min;Detection wavelength is 324nm;Mobile phase:0.3% formic acid solution A, acetonitrile B, gradient elution;Sample size 2mL.
3. the method for preparing chlorogenic acid monomer in the potato according to claim 2 from Black King Kong, which is characterized in that described
Gradient elution is with the following method:0~13min, 70~80%A;13~21min, 65~70%A;21~30min, 70~
80%A.
4. the method for preparing chlorogenic acid monomer in the potato according to claim 1 from Black King Kong, which is characterized in that step
First solution of chlorogenic acid described in S3 and the volume ratio of ethyl acetate are 1:1~2.
5. the method for preparing chlorogenic acid monomer in the potato according to claim 1 from Black King Kong, which is characterized in that described
Macroporous resin adsorption column is any one of AB-8 types, D101 types, DM130 types or X-5 type macroreticular resins in step S2.
6. the method for preparing chlorogenic acid monomer in the potato according to claim 1 from Black King Kong, which is characterized in that step
Ethanol solution elutes chlorogenic acid with the flow velocity of 1~3mL/min in S2, and the volume fraction of the ethanol solution is 60~80%.
7. the method for preparing chlorogenic acid monomer in the potato according to claim 1 from Black King Kong, which is characterized in that described
Step S1 prepares chlorogenic acid extracting solution specifically with the following method:Extracting solution is added into Black King Kong potato powder, 50~
After extracting 1~2h at 70 DEG C, leaching liquor is centrifuged, chlorogenic acid extracting solution is obtained.
8. the method for preparing chlorogenic acid monomer in the potato according to claim 1 or claim 7 from Black King Kong, which is characterized in that
The solid-liquid ratio of Black King Kong potato powder and extracting solution is 1g in step S1:60~80mL.
9. the method for preparing chlorogenic acid monomer in the potato according to claim 8 from Black King Kong, which is characterized in that described
Extracting solution is the hydrochloric acid solution of a concentration of 0.1~0.3mol/L or the citric acid solution of a concentration of 2~4wt%.
10. the method for preparing chlorogenic acid monomer in the potato according to claim 7 from Black King Kong, which is characterized in that step
Suddenly S1 further includes:After cleaning peeling without rotten Black King Kong potato, cut into inch strips, potato slices are dried at 40~50 DEG C,
It is crushed after drying, crosses 40~80 mesh sieve, obtain Black King Kong potato powder.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109809996A (en) * | 2019-02-19 | 2019-05-28 | 西昌学院 | A method of preparing high-purity chlorogenic acid from jacket |
CN109809996B (en) * | 2019-02-19 | 2021-09-24 | 西昌学院 | Method for preparing chlorogenic acid from potato peels |
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