CN116332822A - Method for preparing low-chroma 5-hydroxytryptophan from garna seeds - Google Patents
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- LDCYZAJDBXYCGN-VIFPVBQESA-N 5-hydroxy-L-tryptophan Chemical compound C1=C(O)C=C2C(C[C@H](N)C(O)=O)=CNC2=C1 LDCYZAJDBXYCGN-VIFPVBQESA-N 0.000 title claims abstract description 37
- LDCYZAJDBXYCGN-UHFFFAOYSA-N oxitriptan Natural products C1=C(O)C=C2C(CC(N)C(O)=O)=CNC2=C1 LDCYZAJDBXYCGN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229940000681 5-hydroxytryptophan Drugs 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011347 resin Substances 0.000 claims abstract description 34
- 229920005989 resin Polymers 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 235000000885 Garcinia xanthochymus Nutrition 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000003480 eluent Substances 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 241000593508 Garcinia Species 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 239000003651 drinking water Substances 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims description 2
- 239000002918 waste heat Substances 0.000 claims description 2
- 235000012206 bottled water Nutrition 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 9
- 230000008025 crystallization Effects 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 8
- 239000003463 adsorbent Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000010413 mother solution Substances 0.000 abstract description 2
- 244000119461 Garcinia xanthochymus Species 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 238000004042 decolorization Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 235000020188 drinking water Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000219726 Griffonia simplicifolia Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000001430 anti-depressive effect Effects 0.000 description 1
- 230000002180 anti-stress Effects 0.000 description 1
- 239000000935 antidepressant agent Substances 0.000 description 1
- 229940005513 antidepressants Drugs 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 230000000147 hypnotic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012898 sample dilution Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Saccharide Compounds (AREA)
Abstract
The invention relates to a method for preparing low-chroma 5-hydroxytryptophan from garna seeds. The method comprises the following steps: countercurrent extraction of the garcinia seeds with water, cooling and centrifuging to obtain centrifugate; the centrifugate is adsorbed by macroporous adsorption resin column, the lower column liquid is discarded, and the macroporous adsorption resin column is washed to be colorless and eluted; concentrating the eluent, centrifuging to remove residues, diluting, purifying with macroporous adsorbent resin column, washing macroporous adsorbent resin column with weak acid water, and collecting lower column liquid and water washing liquid; concentrating the collected decolorized solution, crystallizing, filtering, regulating pH of the mother solution to weak acidity, stirring for crystallization, filtering, and drying. The method adopts countercurrent extraction to extract 5-HTP from the garna seeds with water, reduces the extraction times of solvent, realizes continuous extraction, has higher and more stable concentration of 5-HTP in the discharged liquid, and is beneficial to resin adsorption purification.
Description
Technical Field
The invention belongs to the field of extraction and purification of plant active ingredients, and particularly relates to a method for preparing low-chroma 5-hydroxytryptophan from garna seeds.
Background
The garna seed is a dried seed of a tropical leguminous shrub garna grain Griffonia simplicifolia. In african gana, dogo and other western africans, such gana grains have been planted, and gana seeds have been used for treating various diseases since ancient times. The research shows that the main substance with the drug effect is 5-hydroxytryptophan (5-HTP), the content of the main substance in the seeds is very high, and the main substance has physiological effects of antidepressant, central analgesic, hypnotic, anti-stress, endocrine regulation and the like. Some European countries have classified 5-HTP as a pharmaceutical active ingredient and are marketed as a dietary supplement in the United states, the United kingdom, and Canadian. Therefore, garna seed is an important raw material for extracting 5-HTP.
As one of the water-soluble amino acids, 5-HTP is excellent in water solubility, and its solubility in water is 5.5g/100mL (100 ℃ C.) or 1.0g/100mL (5 ℃ C.), so that water is a conventional solvent for extracting 5-HTP. When the acid-base properties in water are different, the existence form of 5-HTP is different (the structural formula is shown below), so that the solubility in water and other properties are affected, and the special properties can be utilized for extraction, purification and decolorization. When the isoelectric point is near the isoelectric point under the regulation of weak acid, the 5-HTP exists mainly in molecular form and in the equilibrium state of amphoteric ions, so that the water solubility is low; when the solution is in a stronger acid or alkaline condition, the solution exists mainly in an ionic form, so that the solubility is greatly improved.
The traditional process for producing 5-HTP from garna seeds is degreasing, extracting, removing impurities, crystallizing, recrystallizing, and finally obtaining high-purity 5-HTP, such as Chinese patent CN1760182A, chinese patent CN101648900A and Chinese patent CN102093281. The traditional process uses supercritical carbon dioxide extraction or other organic solvent extraction methods to remove grease, has higher equipment cost, stricter requirements on technicians and is not friendly to the environment.
In recent years, some new production methods of 5-HTP remove the degreasing step, directly adopt water extraction, such as Chinese patent CN102219726A, but adopt an ultrasonic extraction mode, and in order to improve the impurity removal effect on the water extract, an ultrafiltration membrane of 0.45 μm is added after the filtration of a 60-mesh filter screen, so that the energy consumption of the process is greatly improved, and the production is not facilitated.
Chinese patent CN102464602a discloses a process for acid water extraction, twice purification of ion exchange resin and macroporous adsorption resin, and decolorizing with activated carbon. The process method needs to use chemical reagents with strong pungent smell such as sodium metabisulfite, ammonia water and the like; the ion exchange resin is used for directly adsorbing untreated water extract, so that serious pollution is easily caused to the ion exchange resin, and the problem of difficult recycling is caused; the amount of the used activated carbon is large, the mass ratio of the activated carbon to the garcinia seed raw material is up to 6%, the consumable cost is increased, and meanwhile, the solid waste of the activated carbon is increased.
The color of the 5-HTP products naturally extracted in the market at present mainly comprises white-like color and gray color, and the chromaticity can reach pure white color, and only products produced by biological fermentation technology. The safety of the biologically fermented products is still questionable, and the application field is mainly natural extraction products.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing low-chroma 5-hydroxytryptophan from gana seeds, which aims to overcome the defects of complex process, high cost, unfriendly environment and high chroma of extracting 5-hydroxytryptophan from gana seeds in the prior art.
The invention provides a method for preparing 5-hydroxytryptophan from gana seeds, which comprises the following steps:
(1) Countercurrent extraction of the garcinia seeds with water, cooling the obtained discharged liquid, centrifuging and deslagging to obtain a centrifugate;
(2) Adsorbing the centrifugate in the step (1) by using a macroporous adsorption resin column, discarding the lower column liquid, washing the macroporous adsorption resin column until the macroporous adsorption resin column is colorless, and then eluting;
(3) Concentrating the eluent in the step (2), centrifuging to remove residues, diluting, adsorbing and decoloring through a macroporous adsorption resin column, washing the macroporous adsorption resin column with weak acid water, and collecting column discharging liquid and washing liquid;
(4) Concentrating, crystallizing, filtering, regulating the pH of the mother liquor to be weak acid, stirring, crystallizing, filtering, and drying the obtained crystal to obtain the 5-hydroxytryptophan.
Preferably, the water in the step (1) is drinking water.
Preferably, the water temperature used for countercurrent extraction in the step (1) is 88-92 ℃.
Preferably, the rotation period of the counter-current extractor of the counter-current extraction in the step (1) is 3.0-5.0 hours.
Preferably, the ratio of water to gana seeds in the step (1) is 10-15L: 1kg.
Preferably, the cooling in the step (1) is cooling by recovering waste heat by using a heat exchanger.
Preferably, in the step (2), an ethanol solution is adopted for elution, the volume of the ethanol solution is 3-5 times of the volume of the macroporous adsorption resin column, and the volume fraction of the ethanol solution is 10% -40%.
Preferably, the ratio of the eluent concentrated in the step (3) to the gana seeds in the step (1) is 1-3L: 1kg.
Preferably, the dilution in the step (3) is performed by weak acidic water.
Preferably, the weakly acidic water is an aqueous hydrochloric acid solution.
Preferably, the ratio of the diluted solution in the step (3) to the gana seed in the step (1) is 5-10 l:1kg.
Preferably, the weak acid water in the step (3) is hydrochloric acid water solution.
Preferably, the decolorized solution in the step (4) is concentrated to 1/10-1/15 of the original volume.
Preferably, the mother liquor in the step (4) is adjusted to be weak acid by using sodium hydroxide aqueous solution.
Preferably, the mother liquor in step (4) is adjusted to a pH of 4-6.
Advantageous effects
(1) According to the invention, the countercurrent extraction mode is adopted to extract the 5-HTP from the garcinia seeds by using water, so that the solvent extraction amount is reduced, the continuous extraction is realized, the concentration of the 5-HTP in the discharged liquid is higher and more stable, and the resin adsorption purification is facilitated;
(2) The macroporous resin which is easy to recycle is adopted for purification and decolorization (such as the purification of the polar XDA-8G resin and the decolorization of the nonpolar D101 resin), so that the problem of solid waste caused by decolorization by using activated carbon is avoided, and the method is more environment-friendly;
(3) The existing forms and water solubility of 5-HTP and impurities are changed by regulating the acid and the alkali by using common hydrochloric acid and sodium hydroxide, so that the purification, decolorization and crystallization effects are improved in an auxiliary way, the chromaticity of the obtained product is lower, and the limitation in the application of subsequent products is reduced;
(4) The raw material garcinia seeds are directly adopted, and are not crushed, so that only small molecules can migrate into a solvent from the interior of the garcinia seeds, impurities are reduced, and the water countercurrent extraction at the temperature of 88-92 ℃ is adopted, so that not only is the solubility improved, but also the molecular activity is increased, and 5-HTP can migrate out of the interior of the garcinia seeds more quickly.
Drawings
FIG. 1 is an HPLC chart of a 5-HTP standard sample.
FIG. 2 is an HPLC chart of the product of example 1 of the present invention.
FIG. 3 is an HPLC chart of the product of example 2 of the present invention.
FIG. 4 is an HPLC chart of the product of example 3 of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it will be understood that various changes or modifications may be made by those skilled in the art after reading the teachings of the invention, and such equivalents are intended to fall within the scope of the invention as defined herein.
The method for detecting the content of the 5-HTP by using the HPLC method comprises the following steps: (1) Preparing a 5-HTP standard sample solution (reference solution), (2) preparing a test sample solution; (3) Respectively taking a standard substance solution and a sample solution, injecting the standard substance solution and the sample solution into a liquid chromatograph, recording a chromatogram, calculating the content according to an external standard method by using a peak area, and calculating the content of 5-HTP according to the following calculation formula:
wherein: a is that Sample -sample peak area; a is that For a pair of -control peak area;
W for a pair of -control weighing (mg); w (W) Sample -weighing the test sample (mg);
V sample -dilution factor (ml) of the test sample; v (V) For a pair of -dilution of control (ml);
p-control content (%).
The RSD value of the two detection results must not exceed 2%.
Example 1
Taking 1500kg of gana seeds, extracting the gana seeds in a horizontal rotation type countercurrent extractor by 18000L of drinking water with the temperature of 88-92 ℃ and setting the rotation period of the extractor to be 3.2 hours; cooling the discharged material liquid, centrifuging to remove residues, and adsorbing with 3000L volume XDA-8G macroporous resin; the resin column is washed with 1800L of water and then analyzed by using 9000L of 25 percent ethanol, the ethanol is recovered from the analysis liquid by adopting a reduced pressure distillation mode until the volume is about 1500L, acid water (0.2 percent by volume of industrial hydrochloric acid is added to each part of water) is added to dilute the analysis liquid to 7500L, the resin column is decolorized by 100L of D101 macroporous adsorption resin, 500L of acid water is used for washing, the lower column liquid and the water washing liquid are collected and concentrated to 600L, the crystallization is placed, the mother solution is filtered, the sodium hydroxide aqueous solution with the concentration of 10 percent is added while stirring and crystallization are carried out, the pH is adjusted to 4.5, the stirring is continued for about 2 hours, the crystal is filtered, the solid obtained by the two crystallization is mixed and dried, and the powder is crushed, so that the final product is white 5-HTP, and the content is 99.4 percent by an HPLC method and the yield is 77.9 percent.
Example 2
Taking 1500kg of gana seeds, extracting the gana seeds in a horizontal rotation type countercurrent extractor by 16500L of drinking water with the temperature of 88-92 ℃ and setting the rotation period of the extractor to be 4.5 hours; cooling the discharged material liquid, centrifuging to remove residues, and adsorbing with 2800L volume of XDA-8G macroporous resin; washing the resin column with 1500L of water, resolving with 25% ethanol 9000L, recovering ethanol from the resolving solution by vacuum distillation until no ethanol exists, diluting to about 1500L by adding acid water (0.2% volume industrial hydrochloric acid is added to each part of water), decolorizing with 100L of D101 macroporous adsorbent resin, washing the resin column with 600L of acid water, collecting lower column liquid and water washing liquid, mixing and concentrating to 600L, standing for crystallization, filtering mother liquor, adding 10% sodium hydroxide aqueous solution, stirring for crystallization, adjusting pH to 5.0, stirring for about 2 hours, filtering out crystals, mixing and drying the twice crystallized solids, and pulverizing to obtain white 5-HTP with content of 98.6% and yield of 86.2%.
Example 3
Taking 1500kg of gana seeds, extracting the gana seeds in a horizontal rotation type countercurrent extractor by using 20000L of drinking water with the temperature of 88-92 ℃ and setting the rotation period of the extractor to be 3.6 hours; cooling the discharged material liquid, centrifuging to remove residues, and adsorbing with 3000L volume XDA-8G macroporous resin; washing a resin column with 1600L of water, resolving with 25% ethanol 9000L, recovering ethanol from the resolved solution by vacuum distillation until the volume is about 1500L, adding acid water (0.2% volume industrial hydrochloric acid is added to each part of water) to dilute the solution to 7500L, decolorizing with 100L of D101 macroporous adsorption resin, washing the resin column with 700L of acid water, collecting lower column liquid and water washing liquid, mixing and concentrating to 600L, standing for crystallization, filtering out mother liquor, adding 10% sodium hydroxide aqueous solution, stirring for crystallization, adjusting pH to 5.5, continuing stirring for about 2 hours, filtering out crystals, mixing and drying the twice crystallized solids, and powdering to obtain a final product which is white 5-HTP with the content of 98.3% and the yield of 91.6%.
The absorbance obtained by ultraviolet-visible spectrum scanning after the products of examples 1 to 3 and the commercially available products were formulated with pure water to 10mg/mL is shown in Table 1.
TABLE 1
Commercial natural-derived 5-HTP products often appear off-white or yellow-white, whereas commercial pure-white 5-HTP products are produced by a biological fermentation process, and it is generally difficult to achieve low-to-pure-white chromaticity of the natural-derived 5-HTP products under cost control. As can be seen from the comparison data of the chromaticity of the product of the method and the commercial gana seed extract product, the absorbance of the product of the method is obviously lower than that of the commercial normal off-white and yellow-white 5-HTP product (natural source) and is lower than or close to that of the commercial pure white product (biological fermentation source) in the wavelength scanning range from 330nm to 800 nm.
Claims (8)
1. A method for preparing 5-hydroxytryptophan from gana seed comprising the steps of:
(1) Countercurrent extraction is carried out on the garcinia seeds by using water, the obtained discharged liquid is cooled, and the residue is removed by centrifugation, so that centrifugate is obtained, wherein the countercurrent extraction adopts the water temperature of 88-92 ℃ and the ratio of water to garcinia seeds is 10-15L: 1kg;
(2) Adsorbing the centrifugate in the step (1) by using a macroporous adsorption resin column, discarding the lower column liquid, washing the macroporous adsorption resin column until the macroporous adsorption resin column is colorless, and then eluting;
(3) Concentrating the eluent in the step (2), centrifuging to remove residues, diluting, adsorbing and decoloring through a macroporous adsorption resin column, washing the macroporous adsorption resin column with weak acid water, and collecting column discharging liquid and washing liquid;
(4) Concentrating, crystallizing, filtering, regulating the pH of the mother liquor to be weak acid, stirring, crystallizing, filtering, and drying the obtained crystal to obtain the 5-hydroxytryptophan.
2. The method of claim 1, wherein the water in step (1) is potable water.
3. The method of claim 1, wherein the cooling in step (1) is cooling by recovering waste heat using a heat exchanger.
4. The method according to claim 1, wherein the elution in the step (2) is performed by using an ethanol solution, the volume of the ethanol solution is 3-5 times of the volume of the macroporous adsorption resin column, and the volume fraction of the ethanol solution is 10% -40%.
5. The method of claim 1, wherein the ratio of the eluent concentrated in step (3) to the gana seed in step (1) is 1-3 l:1kg.
6. The method of claim 1, wherein the dilution in step (3) is dilution with weakly acidic water; the ratio of the diluted solution to the gana seeds in the step (1) is 5-10L: 1kg.
7. The method according to claim 1, wherein the decolorized solution in the step (4) is concentrated to 1/10 to 1/15 of the original volume.
8. The method of claim 1, wherein the mother liquor in step (4) is pH adjusted to 4-6.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117347530A (en) * | 2023-12-04 | 2024-01-05 | 天津玉健生物工程有限公司 | Detection method of plasticizer in vitamin B2 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648900A (en) * | 2009-08-31 | 2010-02-17 | 三明华健生物工程有限公司 | Production process for extracting and preparing high-purity 5-hydroxytryptophan from Griffonia simplicifolia |
| CN102464602A (en) * | 2010-11-19 | 2012-05-23 | 苏州宝泽堂医药科技有限公司 | Method for extracting 5-hydroxytryptophan |
| CN104974074A (en) * | 2015-07-30 | 2015-10-14 | 太阳树（厦门）生物工程有限公司 | Production technique for extracting 5-hydroxytryptophan from griffonia simplicifolia seed |
| CN115403504A (en) * | 2022-08-04 | 2022-11-29 | 李玉山 | Extraction and separation method of 5-hydroxytryptophan |
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| CN117347530A (en) * | 2023-12-04 | 2024-01-05 | 天津玉健生物工程有限公司 | Detection method of plasticizer in vitamin B2 |
| CN117347530B (en) * | 2023-12-04 | 2024-02-13 | 天津玉健生物工程有限公司 | Detection method of plasticizer in vitamin B2 |
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