CN107266308A - The technique that a kind of utilization longan pericarp prepares protocatechuic acid - Google Patents
The technique that a kind of utilization longan pericarp prepares protocatechuic acid Download PDFInfo
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- CN107266308A CN107266308A CN201710596858.2A CN201710596858A CN107266308A CN 107266308 A CN107266308 A CN 107266308A CN 201710596858 A CN201710596858 A CN 201710596858A CN 107266308 A CN107266308 A CN 107266308A
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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Abstract
The invention discloses the technique that a kind of utilization longan pericarp prepares protocatechuic acid, belong to protocatechuic acid preparing technical field, the protocatechuic acid is crushed by longan pericarp, ultrasonic wave extraction, once decolouring, coarse crystallization, secondary decolourization, macroporous absorbent resin separating-purifying, condensing crystallizing, drying and other steps are made.The purity of protocatechuic acid is more than 99.21% made from the technique of the present invention, and can be used as qualitative, quantitative reference substance；The technique of the present invention can effectively extract the protocatechuic acid in longan pericarp, advantageously reduce environmental pollution and the wasting of resources that longan pericarp is caused.
Description
【Technical field】
The invention belongs to protocatechuic acid preparing technical field, and in particular to a kind of utilization longan pericarp prepares the work of protocatechuic acid
Skill.
【Background technology】
1- pi-allyl -3- methylimidazolium chlorides and 1- ethyl-3-methylimidazole Acetate Solutions are in room temperature or nearly room temperature
The lower liquid being made up of completely anions and canons, by specific, volume is relatively large, the asymmetric organic cation of structure and
The relatively small inorganic anion composition of volume.In both the above ionic compound, the active force between zwitterion is coulomb
Power, its size is relevant with the amount of charge and radius of zwitterion, and ionic radius is bigger, and the active force between them is smaller, with
As for fusing point close to room temperature.Because 1- pi-allyl -3- methylimidazolium chlorides and 1- ethyl-3-methylimidazoles acetate have in itself
The incomparable advantage of many conventional solvents, extracts active ingredients can be applied to as green solvent.Utilize 1- allyls
Base -3- methylimidazolium chlorides and 1- ethyl-3-methylimidazoles acetate extract volatile oil, can avoid conventional organic solvents extraction method
Recovery rate is low, and cost is high, the shortcoming of high temperature fragrance component.
Longan pericarp is the mature seed of sapindaceous plant longan, and in addition to Chinese medicine is used on a small quantity, that largely abandons is unused, makes
Into environmental pollution and the wasting of resources.Modern clinical research is found, protocatechuic acid is can extract from longan pericarp, and monomer is white
To brown crystalline powder, modern pharmacology experiment shows that it is to gold-coloured staphylococci, streptococcus, Diplococcus pneumopniae, large intestine bar
Bacterium, Pseudomonas aeruginosa, shigella dysenteriae have obvious inhibitory action, and play the role of to restrain and promote to hinder face healing, therefore exist at present
Clinically be used to burning, infantile pneumonia, bacillary dysentery, acute nephropyelitis, the treatment of acute pancreatitis and certain canker.It is put down simultaneously
Breathe heavily, also there is relevant report eliminating the phlegm, the partial efficacy country such as antidote against snake bite.Protocatechuic acid is not only applicable to medicine intermediate, dyestuff etc.
Also as a kind of analytical reagent.
The report document for extracting protocatechuic acid from longan pericarp at present is less, therefore how to develop the original extracted in longan pericarp
Catechuic acid, reduces environmental pollution and the wasting of resources that longan pericarp is caused, and tool is of great significance.
【The content of the invention】
A kind of utilization longan pericarp that the present invention is provided prepares the technique of protocatechuic acid, to solve current longan pericarp except a small amount of use
In outside Chinese medicine, that largely abandons is unused, causes the problem of environmental pollution and wasting of resources.
To solve above technical problem, the present invention uses following technical matters：
A kind of utilization longan pericarp prepares the technique of protocatechuic acid, comprises the following steps：
S1：Longan pericarp is crushed and sifted out, longan pericarp powder is made；
S2：42-125 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, it is small in temperature
Be beaten under the conditions of -10 DEG C, obtain longan pericarp slurries, by longan pericarp slurries and 6-22 parts of 1- pi-allyl -3- methylimidazolium chlorides,
15-32 parts of 1- ethyl-3-methylimidazoles acetate are well mixed, and are put into extraction flask, are 300-450W, temperature in ultrasonic power
Spend to extract 1.2-1.6h under the conditions of 76-92 DEG C, extract solution is made, adjust the pH value of extract solution to 4.2-5.3, temperature control is
45-52 DEG C, by decolorization and impurity removal by active carbon, a destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 5-6.2 times of body of cream is used in
42-46 DEG C long-pending of water is dissolved, and is carried out extraction 2-3 times using anhydrous ethyl acetate solvent, is continued to use anhydrous ethyl acetate
It is 1 to carry out solid-to-liquid ratio in 2-3 crystallization treatment, crystallization process:4.5-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 65%-75%, the pH value of solution is adjusted to 4.5-5.8, it is warm
Degree control is 45-58 DEG C, by decolorization and impurity removal by active carbon, and secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into B3%-10% containing compound in every milliliter, inhaled using macropore
Compound B liquid is made in attached resin separating-purifying, and condition is：The ethanol solution that agent is 46%-58% is parsed, its consumption is big
1.8-3.2 times of macroporous adsorbent resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is 2.8%-
5.6% KOH solution, adsorption zone flow velocity 6-10BV/h, desorption zone flow velocity 10-20BV/h, water wash zone flow velocity 20-25BV/h, then
Raw area flow velocity 6-10BV/h, switching time is 700-750s, and temperature is 43-52 DEG C, and pressure is 0.5-0.8MPa；
S6：Crystallized after compound B liquid made from step S5 is concentrated, gained crystal is in the case where temperature is 40-45 DEG C
Vacuum drying, is made compound B, and it is protocatechuic acid to determine compound B through the analysis of HPLC methods.
Preferably, the mesh number of sieve described in step S1 is 30-80.
Preferably, ultrasonic wave extraction condition described in step S2：Power is 450W, and temperature is extraction under the conditions of 92 DEG C
1.2h。
Preferably, the pH value of extract solution is adjusted described in step S2 to 5.2.
Preferably, it is 0.9-1.6h by the time of decolorization and impurity removal by active carbon described in step S2.
Preferably, it is 0.6-1.2h by the time of decolorization and impurity removal by active carbon described in step S4.
Preferably, macroporous absorbent resin described in step S5 is H-103 type macroporous absorbent resins.
Preferably, concentration described in step S6 is vacuum-concentrcted.
Preferably, crystallization described in step S6 is carried out in the case where temperature is 3-7 DEG C.
Preferably, crystal described in step S6 is dried under vacuum to moisture content≤0.8% in the case where temperature is 40-43 DEG C.
The invention has the advantages that：
(1) purity of protocatechuic acid made from technique of the invention is more than 99.21%, and can be as qualitative, quantitative
Reference substance；
(2) technique of the invention can effectively extract the protocatechuic acid in longan pericarp, advantageously reduce the ring that longan pericarp is caused
Pollute and the wasting of resources in border.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following examples, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In embodiment, the utilization longan pericarp prepares the technique of protocatechuic acid, comprises the following steps：
S1：Longan pericarp is crushed and 30-80 mesh sieve is crossed, longan pericarp powder is made；
S2：42-125 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, it is small in temperature
Be beaten under the conditions of -10 DEG C, obtain longan pericarp slurries, by longan pericarp slurries and 6-22 parts of 1- pi-allyl -3- methylimidazolium chlorides,
15-32 parts of 1- ethyl-3-methylimidazoles acetate are well mixed, and are put into extraction flask, are 300-450W, temperature in ultrasonic power
Spend to extract 1.2-1.6h under the conditions of 76-92 DEG C, extract solution is made, adjust the pH value of extract solution to 4.2-5.3, temperature control is
45-52 DEG C, by decolorization and impurity removal by active carbon 0.9-1.6h, a destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 5-6.2 times of body of cream is used in
42-46 DEG C long-pending of water is dissolved, and is carried out extraction 2-3 times using anhydrous ethyl acetate solvent, is continued to use anhydrous ethyl acetate
It is 1 to carry out solid-to-liquid ratio in 2-3 crystallization treatment, crystallization process:4.5-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 65%-75%, the pH value of solution is adjusted to 4.5-5.8, it is warm
Degree control is 45-58 DEG C, by decolorization and impurity removal by active carbon 0.6-1.2h, and secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into B3%-10% containing compound in every milliliter, using H-103
Compound B liquid is made in type macroporous absorbent resin separating-purifying, and condition is：The ethanol solution that agent is 46%-58% is parsed, its
Consumption is 1.8-3.2 times of macroporous absorbent resin volume, and water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is
2.8%-5.6% KOH solution, adsorption zone flow velocity 6-10BV/h, desorption zone flow velocity 10-20BV/h, water wash zone flow velocity 20-
25BV/h, renewing zone flow velocity 6-10BV/h, switching time are 700-750s, and temperature is 43-52 DEG C, and pressure is 0.5-0.8MPa；
S6：Compound B liquid made from step S5 is carried out after vacuum-concentrcted, tied in the case where temperature is 3-7 DEG C
Crystalline substance, gained crystal is dried under vacuum to moisture content≤0.8% in the case where temperature is 40-43 DEG C, and compound B is made.
Embodiment 1
A kind of utilization longan pericarp prepares the technique of protocatechuic acid, comprises the following steps：
S1：Longan pericarp is crushed and 60 mesh sieve are crossed, longan pericarp powder is made；
S2：85 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, are -12 DEG C in temperature
Under the conditions of be beaten, obtain longan pericarp slurries, by longan pericarp slurries and 14 parts of 1- pi-allyl -3- methylimidazolium chlorides, 25 parts of 1- ethyls -
3- methylimidazoles acetate is well mixed, and is put into extraction flask, is 400W in ultrasonic power, temperature is extraction under the conditions of 86 DEG C
1.5h, is made extract solution, adjusts the pH value of extract solution to 4.6, temperature control is 50 DEG C, by decolorization and impurity removal by active carbon 1.3h,
A destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 5.6 times of volumes of cream are used in
45 DEG C of water dissolved, using anhydrous ethyl acetate solvent carry out extraction 2 times, continuation is carried out 2 times with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystallization treatment, crystallization process:4.8W/V), crystal crude product is made；
S4：Coarse-grain made from step S3 is dissolved through 70% ethanol, the pH value of solution is adjusted to 5.2, temperature control is
53 DEG C, by decolorization and impurity removal by active carbon 0.9h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into B7% containing compound in every milliliter, using H-103 type macropores
Compound B liquid is made in polymeric adsorbent separating-purifying, and condition is：The ethanol solution that agent is 52% is parsed, its consumption is macropore
2.5 times of polymeric adsorbent volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is molten for 4.2% KOH
Liquid, adsorption zone flow velocity 8BV/h, desorption zone flow velocity 15BV/h, water wash zone flow velocity 22BV/h, renewing zone flow velocity 8BV/h, switching time
For 730s, temperature is 48 DEG C, and pressure is 0.7MPa；
S6：Compound B liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 6 DEG C,
Gained crystal is that to be dried under vacuum to moisture content at 42 DEG C be 0.8% in temperature, and compound B is made.
Embodiment 2
A kind of utilization longan pericarp prepares the technique of protocatechuic acid, comprises the following steps：
S1：Longan pericarp is crushed and 30 mesh sieve are crossed, longan pericarp powder is made；
S2：43 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, are -10 DEG C in temperature
Under the conditions of be beaten, obtain longan pericarp slurries, by longan pericarp slurries and 7 parts of 1- pi-allyl -3- methylimidazolium chlorides, 15 parts of 1- ethyls -
3- methylimidazoles acetate is well mixed, and is put into extraction flask, is 300W in ultrasonic power, temperature is extraction under the conditions of 76 DEG C
1.6h, is made extract solution, adjusts the pH value of extract solution to 4.2, temperature control is 46 DEG C, by decolorization and impurity removal by active carbon 1.6h,
A destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 5 times of volumes of cream are used in
42 DEG C of water is dissolved, and extraction 2 times is carried out using anhydrous ethyl acetate solvent, and continuation carries out 2 knots with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystalline substance processing, crystallization process:4.5 (W/V), are made crystal crude product；
S4：Coarse-grain made from step S3 is dissolved through 65% ethanol, the pH value of solution is adjusted to 4.5, temperature control is
45 DEG C, by decolorization and impurity removal by active carbon 1.2h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into B4% containing compound in every milliliter, using H-103 type macropores
Compound B liquid is made in polymeric adsorbent separating-purifying, and condition is：The ethanol solution that agent is 46% is parsed, its consumption is macropore
1.8 times of polymeric adsorbent volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is molten for 2.8% KOH
Liquid, adsorption zone flow velocity 6BV/h, desorption zone flow velocity 10BV/h, water wash zone flow velocity 20BV/h, renewing zone flow velocity 6BV/h, switching time
For 750s, temperature is 43 DEG C, and pressure is 0.5MPa；
S6：Compound B liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 3 DEG C,
Gained crystal is that to be dried under vacuum to moisture content at 40 DEG C be 0.7% in temperature, and compound B is made.
Embodiment 3
A kind of utilization longan pericarp prepares the technique of protocatechuic acid, comprises the following steps：
S1：Longan pericarp is crushed and 80 mesh sieve are crossed, longan pericarp powder is made；
S2：123 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, are -15 DEG C in temperature
Under the conditions of be beaten, obtain longan pericarp slurries, by longan pericarp slurries and 20 parts of 1- pi-allyl -3- methylimidazolium chlorides, 30 parts of 1- ethyls -
3- methylimidazoles acetate is well mixed, and is put into extraction flask, is 450W in ultrasonic power, temperature is extraction under the conditions of 92 DEG C
1.2h, is made extract solution, adjusts the pH value of extract solution to 5.3, temperature control is 52 DEG C, by decolorization and impurity removal by active carbon 0.9h,
A destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 6.2 times of volumes of cream are used in
46 DEG C of water dissolved, using anhydrous ethyl acetate solvent carry out extraction 3 times, continuation is carried out 3 times with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystallization treatment, crystallization process:4.9 (W/V), are made crystal crude product；
S4：Coarse-grain made from step S3 is dissolved through 75% ethanol, the pH value of solution is adjusted to 5.8, temperature control is
58 DEG C, by decolorization and impurity removal by active carbon 0.6h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into every milliliter and contains compound B-11 0%, it is big using H-103 types
Compound B liquid is made in macroporous adsorbent resin separating-purifying, and condition is：The ethanol solution that agent is 58% is parsed, its consumption is big
3.2 times of macroporous adsorbent resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is molten for 5.6% KOH
Liquid, adsorption zone flow velocity 10BV/h, desorption zone flow velocity 20BV/h, water wash zone flow velocity 25BV/h, renewing zone flow velocity 10BV/h, during switching
Between be 700, temperature be 52 DEG C, pressure is 0.8MPa；
S6：Compound B liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 6 DEG C,
Gained crystal is that to be dried under vacuum to moisture content at 43 DEG C be 0.6% in temperature, and compound B is made.
Below by taking embodiment 1 as an example, the measure technique to compound B is described in detail：
First, TLC methods (thin-layered chromatography)：
(1) prepared by reference substance solution：Precision weighs protocatechuic acid reference substance, and its purity is more than 99%, plus methanol is made
Per solution of the 1ml containing 0.5mg, reference substance solution is used as.
(2) prepared by need testing solution：Take compound B, plus proper amount of methanol to make dissolving, be used as need testing solution.
(3) differentiate：Tested with reference to one B of annex VI of China's coastal port, draw need testing solution and control
Each 10 μ l of product solution, put on upper same silica gel g thin-layer plate, using chloroform-acetone-methanol as 6 respectively:1:1 proportions it is molten
Liquid deploys as solvent, takes out, dries, put and inspected under ultraviolet lamp (256nm), in test sample chromatogram, with control medicinal material
On the relevant position of chromatogram and reference substance chromatogram, show the spot of same color.
(4) result：It is protocatechuic acid that thin-layer chromatography inspection, which determines compound B,.
2nd, HPLC methods (high performance liquid chromatography (HPLC))
(1) instrument and reagent
High performance liquid chromatograph：Japanese Shimadzu LC-6A, performance liquid chromatographic column：Chinese Academy of Sciences's Dalian Chemical Physics is ground
Study carefully institute's product, 4.6 × 250mm of Ф, filler is Nucleosil7C18, ultraviolet 256nm detections.
(2) method
1) chromatographic condition：Performance liquid chromatographic column Nucleosil7C18 (4.6 × 250mm of Ф), mobile phase is methanol -1%
Glacial acetic acid solution (8:95, v/v), flow velocity is 1ml/min, and column temperature is detection under room temperature, Detection wavelength 256nm, and number of theoretical plate is former
Catechuic acid peak should be not less than 4000.
2) preparation of reference substance solution and need testing solution will not be repeated here with TLC methods.
3) Precision Experiment draws reference substance and each 10 μ l of need testing solution, injects high performance liquid chromatograph, determines former youngster
The content of boheic acid, it is protocatechuic acid to determine compound B.
(3) result：The time consistency retained with protocatechuic acid reference substance is determined through HPLC, white crystal, fusing point is 200-
202 DEG C, combined according to data analysis with document, it is protocatechuic acid to determine compound B.
Shown by embodiment 1, the present invention prepares the technique of protocatechuic acid using longan pericarp, reliably, and DNA purity is high,
Same experiment is made with embodiment 2,3, close effect is similarly reached.
The purity of protocatechuic acid made from embodiment 1-3 is detected using HPLC methods, it is as a result as shown in the table.
From with upper table, the purity of protocatechuic acid made from technique of the invention can be used as calmly more than 99.21%
Property, quantitative reference substance.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations, for person of an ordinary skill in the technical field, is not departing from
On the premise of present inventive concept, some simple deduction or replace can also be made, the present invention should be all considered as belonging to by being submitted
Claims determine scope of patent protection.
Claims (10)
1. the technique that a kind of utilization longan pericarp prepares protocatechuic acid, it is characterised in that comprise the following steps：
S1：Longan pericarp is crushed and sifted out, longan pericarp powder is made；
S2：42-125 parts of longan pericarp powder made from step S1 are weighed, technology is beaten using low temperature liquid nitrogen, are less than -10 in temperature
Be beaten under the conditions of DEG C, obtain longan pericarp slurries, by longan pericarp slurries and 6-22 parts of 1- pi-allyl -3- methylimidazolium chlorides, 15-32 parts
1- ethyl-3-methylimidazoles acetate is well mixed, and is put into extraction flask, is 300-450W in ultrasonic power, temperature is 76-
1.2-1.6h is extracted under the conditions of 92 DEG C, extract solution is made, the pH value of extract solution is adjusted to 4.2-5.3, temperature control is 45-52
DEG C, by decolorization and impurity removal by active carbon, a destainer is made after filtering；
S3：A destainer made from step S2 is concentrated and dried, extraction cream is made, extraction 5-6.2 times of volume of cream is used in
42-46 DEG C of water is dissolved, and carries out extraction 2-3 times using anhydrous ethyl acetate solvent, continuation is carried out with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in 2-3 crystallization treatment, crystallization process:4.5-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 65%-75%, the pH value of solution is adjusted to 4.5-5.8, temperature control
45-58 DEG C is made as, by decolorization and impurity removal by active carbon, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into B3%-10% containing compound in every milliliter, using macroporous absorption tree
Compound B liquid is made in fat separating-purifying, and condition is：The ethanol solution that agent is 46%-58% is parsed, its consumption is that macropore is inhaled
1.8-3.2 times of attached resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is 2.8%-5.6%
KOH solution, adsorption zone flow velocity 6-10BV/h, desorption zone flow velocity 10-20BV/h, water wash zone flow velocity 20-25BV/h, renewing zone stream
Fast 6-10BV/h, switching time is 700-750s, and temperature is 43-52 DEG C, and pressure is 0.5-0.8MPa；
S6：Crystallized after compound B liquid made from step S5 is concentrated, gained crystal vacuum in the case where temperature is 40-45 DEG C
Dry, compound B is made, it is protocatechuic acid to determine compound B through the analysis of HPLC methods.
2. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S1
The mesh number of sieve is 30-80.
3. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S2
Ultrasonic wave extraction condition：Power is 450W, and temperature is to extract 1.2h under the conditions of 92 DEG C.
4. the technique that utilization longan pericarp according to claim 3 prepares protocatechuic acid, it is characterised in that：Described in step S2
The pH value of extract solution is adjusted to 5.2.
5. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S2
Time by decolorization and impurity removal by active carbon is 0.9-1.6h.
6. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S4
Time by decolorization and impurity removal by active carbon is 0.6-1.2h.
7. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S5
Macroporous absorbent resin is H-103 type macroporous absorbent resins.
8. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S6
Concentrate as vacuum-concentrcted.
9. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Described in step S6
Crystallization is carried out in the case where temperature is 3-7 DEG C.
10. the technique that utilization longan pericarp according to claim 1 prepares protocatechuic acid, it is characterised in that：Institute in step S6
State crystal and be dried under vacuum to moisture content≤0.8% in the case where temperature is 40-43 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739307A (en) * | 2017-10-31 | 2018-02-27 | 中国农业大学 | A kind of dilute alkaline soln extraction solid-phase extraction column purifies the method for protocatechuic acid |
| CN109856254A (en) * | 2018-01-11 | 2019-06-07 | 广西中医药大学 | The method for building up and its finger-print of longan leaf ethyl acetate extract HPLC finger-print |
| CN112047828A (en) * | 2020-09-04 | 2020-12-08 | 宜昌东阳光生化制药有限公司 | Method for preparing protocatechuic acid by biochemical method |
| CN112142591A (en) * | 2020-10-09 | 2020-12-29 | 中国科学院天津工业生物技术研究所 | Method for separating and extracting protocatechuic acid from fermentation liquor |
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| CN112142591A (en) * | 2020-10-09 | 2020-12-29 | 中国科学院天津工业生物技术研究所 | Method for separating and extracting protocatechuic acid from fermentation liquor |
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