CN114621304A - Process for extracting gastrodin - Google Patents
Process for extracting gastrodin Download PDFInfo
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- CN114621304A CN114621304A CN202210173610.6A CN202210173610A CN114621304A CN 114621304 A CN114621304 A CN 114621304A CN 202210173610 A CN202210173610 A CN 202210173610A CN 114621304 A CN114621304 A CN 114621304A
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- extraction
- gastrodin
- rhizoma gastrodiae
- carbon dioxide
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- PUQSUZTXKPLAPR-UJPOAAIJSA-N Gastrodin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(CO)C=C1 PUQSUZTXKPLAPR-UJPOAAIJSA-N 0.000 title claims abstract description 62
- PUQSUZTXKPLAPR-KSSYENDESA-N 4-(beta-D-Glucopyranosyloxy) benzyl alcohol Natural products O([C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1)c1ccc(CO)cc1 PUQSUZTXKPLAPR-KSSYENDESA-N 0.000 title claims abstract description 53
- 229930193974 gastrodin Natural products 0.000 title claims abstract description 53
- PUQSUZTXKPLAPR-NZEXEKPDSA-N helicidol Natural products O([C@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](CO)O1)c1ccc(CO)cc1 PUQSUZTXKPLAPR-NZEXEKPDSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims description 6
- 238000000605 extraction Methods 0.000 claims abstract description 89
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000000843 powder Substances 0.000 claims abstract description 44
- 108090000790 Enzymes Proteins 0.000 claims abstract description 20
- 102000004190 Enzymes Human genes 0.000 claims abstract description 20
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- KAXSXFHMJDMWOM-UHFFFAOYSA-L dipotassium;hydrogen phosphate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [K+].[K+].OP([O-])([O-])=O.OC(=O)CC(O)(C(O)=O)CC(O)=O KAXSXFHMJDMWOM-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000000284 extract Substances 0.000 claims abstract description 13
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- 230000002255 enzymatic effect Effects 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 26
- 229940088598 enzyme Drugs 0.000 claims description 19
- 241000305491 Gastrodia elata Species 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000004382 Amylase Substances 0.000 claims description 9
- 108010065511 Amylases Proteins 0.000 claims description 9
- 102000013142 Amylases Human genes 0.000 claims description 9
- 108090000526 Papain Proteins 0.000 claims description 9
- 108010059820 Polygalacturonase Proteins 0.000 claims description 9
- 239000004365 Protease Substances 0.000 claims description 9
- 235000019418 amylase Nutrition 0.000 claims description 9
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 9
- 229940059442 hemicellulase Drugs 0.000 claims description 9
- 108010002430 hemicellulase Proteins 0.000 claims description 9
- 229940055729 papain Drugs 0.000 claims description 9
- 235000019834 papain Nutrition 0.000 claims description 9
- 108010059892 Cellulase Proteins 0.000 claims description 8
- 229940106157 cellulase Drugs 0.000 claims description 8
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims 1
- 239000000413 hydrolysate Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 7
- 238000002791 soaking Methods 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- 239000001814 pectin Substances 0.000 description 4
- 229920001277 pectin Polymers 0.000 description 4
- 235000010987 pectin Nutrition 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000002137 ultrasound extraction Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 238000000874 microwave-assisted extraction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- KZJWDPNRJALLNS-VPUBHVLGSA-N (-)-beta-Sitosterol Natural products O[C@@H]1CC=2[C@@](C)([C@@H]3[C@H]([C@H]4[C@@](C)([C@H]([C@H](CC[C@@H](C(C)C)CC)C)CC4)CC3)CC=2)CC1 KZJWDPNRJALLNS-VPUBHVLGSA-N 0.000 description 1
- CSVWWLUMXNHWSU-UHFFFAOYSA-N (22E)-(24xi)-24-ethyl-5alpha-cholest-22-en-3beta-ol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(CC)C(C)C)C1(C)CC2 CSVWWLUMXNHWSU-UHFFFAOYSA-N 0.000 description 1
- KLEXDBGYSOIREE-UHFFFAOYSA-N 24xi-n-propylcholesterol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CCC)C(C)C)C1(C)CC2 KLEXDBGYSOIREE-UHFFFAOYSA-N 0.000 description 1
- LPZCCMIISIBREI-MTFRKTCUSA-N Citrostadienol Natural products CC=C(CC[C@@H](C)[C@H]1CC[C@H]2C3=CC[C@H]4[C@H](C)[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C)C(C)C LPZCCMIISIBREI-MTFRKTCUSA-N 0.000 description 1
- ARVGMISWLZPBCH-UHFFFAOYSA-N Dehydro-beta-sitosterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)CCC(CC)C(C)C)CCC33)C)C3=CC=C21 ARVGMISWLZPBCH-UHFFFAOYSA-N 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- MJVXAPPOFPTTCA-UHFFFAOYSA-N beta-Sistosterol Natural products CCC(CCC(C)C1CCC2C3CC=C4C(C)C(O)CCC4(C)C3CCC12C)C(C)C MJVXAPPOFPTTCA-UHFFFAOYSA-N 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- LJQKCYFTNDAAPC-UHFFFAOYSA-N ethanol;ethyl acetate Chemical compound CCO.CCOC(C)=O LJQKCYFTNDAAPC-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- -1 monomethyl ester Chemical class 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- NLQLSVXGSXCXFE-UHFFFAOYSA-N sitosterol Natural products CC=C(/CCC(C)C1CC2C3=CCC4C(C)C(O)CCC4(C)C3CCC2(C)C1)C(C)C NLQLSVXGSXCXFE-UHFFFAOYSA-N 0.000 description 1
- 235000015500 sitosterol Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a gastrodin extraction process, which comprises the following steps: dissolving rhizoma gastrodiae powder in a citric acid-dipotassium hydrogen phosphate buffer solution, adjusting the pH value to 4.5-7.0, and then adding a complex enzyme accounting for 0.5-1% of the mass of the rhizoma gastrodiae powder to obtain rhizoma gastrodiae powder enzymatic hydrolysate; and step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent and ethanol as an entrainer, extracting at the temperature of 40-65 ℃, under the extraction pressure of 35-70 MPa for 0.5-3 hours, and collecting a gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment. The extraction method of the invention also improves the purity of gastrodin under the conditions of short time consumption and high extraction rate.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, and relates to a gastrodin extraction process.
Background
Gastrodia elata is an orchidaceae plant, dried tubers of Gastrodia elata have more than two thousand years of medicinal history in China, and in the past medical literature and data documents, the chemical components of Gastrodia elata comprise gastrodin, beta 2 sitosterol and D2 glucoside thereof, citric acid and symmetrical monomethyl ester thereof, palmitic acid, sucrose and the like, wherein the gastrodin is the main active component thereof. The gastrodine has small molecular weight, high polarity, and good tranquilizing and sleep improving effects. With the development of artificial culture technology of gastrodia elata in recent years, sufficient medicine sources are provided for extracting gastrodin. The traditional extraction process of gastrodin comprises the following steps: ultrasonic extraction and hot alcohol extraction. The two methods take longer time, and the gastrodin contained in the gastrodia elata cannot be extracted to the maximum extent due to low yield of the gastrodin. Therefore, it is very necessary to develop a gastrodin extraction process with short time and improved extraction rate.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a gastrodin extraction process.
To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a gastrodine extraction process comprising the steps of:
firstly, dissolving rhizoma gastrodiae powder in a citric acid-dipotassium hydrogen phosphate buffer solution, adjusting the pH value to 4.5-7.0, and then adding a complex enzyme which accounts for 0.5-1% of the mass of the rhizoma gastrodiae powder into the buffer solution, wherein the complex enzyme comprises 2-3 parts by weight of cellulase, 1-2 parts by weight of hemicellulase, 1-3 parts by weight of papain, 1-3 parts by weight of pectinase and 1-2 parts by weight of amylase; obtaining rhizoma Gastrodiae powder enzymolysis liquid; the cellulose and the hemicellulase in the invention can effectively degrade the cell wall of the gastrodia elata cell, the pectin and the protein in the gastrodia elata cell can be degraded by the pectinase and the papain, and the amylase can carry out enzymolysis on the starch of the gastrodia elata cell, so that the effective components of the gastrodia elata wrapped by the pectin, the protein, the starch and the like can be completely released.
And step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent and ethanol as an entrainer, extracting at the temperature of 40-65 ℃, under the extraction pressure of 35-70 Mpa for 0.5-3 hours, and finally collecting a gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment. Directly pumping rhizoma Gastrodiae powder added with complex enzyme into supercritical carbon dioxide extraction equipment, and performing enzymolysis while extracting
Preferably, in the gastrodin extraction process, in the first step, the mass-to-volume ratio of the gastrodia elata powder to the citric acid-dipotassium hydrogen phosphate buffer solution is 1: 2-5; the pH value of the solution is adjusted by adopting HCl solution and NaOH solution. So that the pH value of the solution meets the requirement.
Preferably, in the gastrodin extraction process, in the first step, the gastrodin enzymatic hydrolysate is subjected to enzymolysis for 20-60 minutes at the temperature of 40-55 ℃ under the stirring condition, and then the gastrodin is subjected to the second step. The composite enzyme is firstly used for enzymolysis for a period of time to promote the release of the active ingredients of gastrodin.
Preferably, in the gastrodin extraction process, in the second step, CO is added2The flow rate is 15-30 kg/h.
Preferably, in the gastrodin extraction process, in the second step, the extraction comprises two stages, wherein the pressure of the first stage is 35-50 Mpa, the extraction temperature is 40-55 ℃, the extraction time is 0.25-1.5 hours, the pressure of the second stage is 50-70 Mpa, the extraction temperature is 56-65 ℃, and the extraction time is 0.25-1.5 hours. The effective components in the gastrodin are gradually extracted by adopting staged extraction.
Preferably, in the gastrodin extraction process, the amount of ethanol used in the first stage is 0.2-0.5 mL, and the amount of ethanol used in the second stage is 2-3 mL.
Preferably, in the gastrodin extraction process, the volume part of the ethanol is 75-99%.
Preferably, in the gastrodine extraction process, the grain size of the gastrodia elata powder is not larger than 100 meshes.
The invention at least comprises the following beneficial effects:
the cellulase and the hemicellulase in the complex enzyme can effectively degrade the cell wall of the gastrodia elata cell, the pectinase and the papain can degrade pectin and protein in the gastrodia elata cell, and meanwhile, the amylase can carry out enzymolysis on the starch, so that the effective ingredients of the gastrodia elata wrapped by the pectin, the protein, the starch and the like can be completely released, and the effect is mild. The gastrodia elata powder added with the complex enzyme is directly pumped into supercritical carbon dioxide extraction equipment, enzymolysis is carried out while extraction is carried out, and the extraction and the enzymolysis are carried out simultaneously, so that the extraction period of gastrodin is greatly shortened, and the purity of gastrodin is improved under the conditions of short time consumption and high extraction rate.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples to enable those skilled in the art to practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
Example 1
The gastrodin extraction process comprises the following steps:
dissolving rhizoma gastrodiae powder sieved by a 120-mesh sieve in a citric acid-dipotassium hydrogen phosphate buffer solution, wherein the mass volume ratio of the rhizoma gastrodiae powder to the citric acid-dipotassium hydrogen phosphate buffer solution is 1:3.5, adjusting the pH value of the solution to be 5 by adopting an HCl solution and an NaOH solution, and then adding a complex enzyme accounting for 0.75% of the mass of the rhizoma gastrodiae powder into the solution to obtain rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 2.5 parts of cellulase, 1.5 parts of hemicellulase, 2 parts of papain, 2 parts of pectinase and 1.5 parts of amylase in parts by weight.
Step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent, taking 90% ethanol in parts by volume as an entrainer, and CO2The flow rate was 20 kg/h. The extraction temperature is 50 ℃, the extraction pressure is 55Mpa, the extraction time is 2 hours, and the dosage of 90% ethanol is 1.5mL, and finally the gastrodin extract is collected from the separation kettle of the supercritical carbon dioxide extraction equipment.
Example 2
The gastrodin extraction process comprises the following steps:
dissolving rhizoma gastrodiae powder sieved by a 120-mesh sieve in a citric acid-dipotassium hydrogen phosphate buffer solution, wherein the mass-volume ratio of the rhizoma gastrodiae powder to the citric acid-dipotassium hydrogen phosphate buffer solution is 1:2, adjusting the pH value to 4.5 by adopting an HCl solution and an NaOH solution, and then adding a complex enzyme accounting for 0.5% of the mass of the rhizoma gastrodiae powder into the solution to obtain a rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 2 parts of cellulase, 1 part of hemicellulase, 1 part of papain, 1 part of pectinase and 1 part of amylase in parts by weight;
and (3) performing enzymolysis on the gastrodin enzymolysis liquid for 20 minutes at the temperature of 40 ℃ under the stirring condition, and then entering the step two.
And step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid in the step one into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent, ethanol as an entrainer, extracting at 40 ℃, under 35Mpa for 0.5 hour, and finally collecting the gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment. CO 22The flow rate was 15 kg/h. The volume part of the ethanol is 75 percent.
Example 3
The gastrodin extraction process comprises the following steps:
dissolving rhizoma gastrodiae powder sieved by a 120-mesh sieve in a citric acid-dipotassium hydrogen phosphate buffer solution, wherein the mass-volume ratio of the rhizoma gastrodiae powder to the citric acid-dipotassium hydrogen phosphate buffer solution is 1:5, adjusting the pH value to 7.0 by adopting an HCl solution and an NaOH solution, and then adding a complex enzyme accounting for 1% of the mass of the rhizoma gastrodiae powder into the solution to obtain rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 3 parts by weight of cellulase, 2 parts by weight of hemicellulase, 3 parts by weight of papain, 3 parts by weight of pectinase and 2 parts by weight of amylase;
step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid in the step one into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent, taking ethanol as an entrainer and CO2The flow rate was 30 kg/h. The volume part of the ethanol is 99 percent. The extraction comprises two stages, wherein the pressure of the first stage is 50Mpa, the extraction temperature is 55 ℃, the extraction time is 1.5 hours, the pressure of the second stage is 70Mpa, the extraction temperature is 65 ℃, and the extraction time is 1.5 hours. In the first stage, the amount of ethanol is 0.5mL, and in the second stageIn this section, the amount of ethanol used was 3 mL. And finally, collecting the gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment.
Example 4
The gastrodin extraction process comprises the following steps:
dissolving rhizoma gastrodiae powder sieved by a 120-mesh sieve in a citric acid-dipotassium hydrogen phosphate buffer solution, adjusting the pH value to 5.5, and then adding a complex enzyme accounting for 0.75% of the mass of the rhizoma gastrodiae powder into the buffer solution to obtain rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 2.5 parts by weight of cellulase, 1.5 parts by weight of hemicellulase, 1.5 parts by weight of papain, 2 parts by weight of pectinase and 1.5 parts by weight of amylase; and (3) carrying out enzymolysis on the gastrodin enzymolysis liquid at the temperature of 55 ℃ for 60 minutes under the stirring condition, and then entering the step two.
And step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid in the step one into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent and ethanol as an entrainer, wherein the extraction comprises two stages, the pressure in the first stage is 35Mpa, the extraction temperature is 40 ℃, the extraction time is 0.25 hour, the pressure in the second stage is 50Mpa, the extraction temperature is 56 ℃, and the extraction time is 0.25 hour. In the first stage, the amount of ethanol was 0.2mL, and in the second stage, the amount of ethanol was 2 mL. And finally, collecting the gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment. CO 22The flow rate was 15 kg/h. The volume part of the ethanol is 75 percent.
Example 5
The gastrodin extraction process comprises the following steps:
dissolving rhizoma gastrodiae powder sieved by a 120-mesh sieve in a citric acid-dipotassium hydrogen phosphate buffer solution, adjusting the pH value to be 5, and then adding a complex enzyme accounting for 0.75% of the mass of the rhizoma gastrodiae powder into the buffer solution to obtain rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 2 parts by weight of cellulase, 1-2 parts by weight of hemicellulase, 1-3 parts by weight of papain, 1-3 parts by weight of pectinase and 1-2 parts by weight of amylase; and (3) performing enzymolysis on the gastrodin enzymatic hydrolysate for 40 minutes at the temperature of 48 ℃ under the stirring condition, and then entering the second step.
Step (ii) ofSecondly, directly adding the rhizoma gastrodiae powder enzymolysis liquid in the step one into a supercritical carbon dioxide extraction device for extraction, wherein carbon dioxide is used as a solvent, ethanol is used as an entrainer, and CO is used2The flow rate was 23 kg/h. The volume part of the ethanol is 90 percent. The extraction comprises two stages: the pressure of the first stage is 42Mpa, the extraction temperature is 48 ℃, the dosage of ethanol is 0.3mL, and the extraction time is 0.9 hour; and in the second stage, the pressure is 60Mpa, the extraction temperature is 62 ℃, the extraction time is 1.2 hours, the dosage of ethanol is 2.5mL, and gastrodin extract is collected from a separation kettle of the supercritical carbon dioxide extraction equipment.
Comparative example 1
Sieving dried rhizoma Gastrodiae powder with 120 mesh sieve, adding ethanol solution, mixing, and soaking, wherein the concentration of ethanol solution is 65%; the mass ratio of the gastrodia elata powder to the ethanol is 1: 20.5; soaking for 200min at 28 deg.C;
sequentially performing microwave extraction (microwave extraction power is 450W, temperature is 45 ℃, time is 25min), ultrasonic extraction (ultrasonic extraction power is 300W, frequency is 45kHz, temperature is 45 ℃, action is 3min and is stopped for 2min, total extraction time is 20min each time), filtering, adding ethanol solution into filter residue for soaking, repeating the above extraction operation twice, and combining filtrates to obtain an extract; drying the above extractive solution to obtain gastrodin extract.
Comparative example 2
Sieving dried rhizoma Gastrodiae powder with 120 mesh sieve, adding ethanol extraction solvent, and soaking for 12 hr to obtain soaking solution; injecting the soaking solution into an ultrasonic water bath heating device for extraction for 2-4 times (30-120 min/time) to obtain extractive solution; filtering the extractive solution, centrifuging, collecting supernatant, filtering with microporous membrane, and collecting filtrate to obtain crude gastrodin extractive solution; and (3) loading the crude gastrodin extract to a macroporous resin chromatographic column, eluting by using an ethanol-ethyl acetate mixed solvent to obtain an eluent, and drying the eluent to obtain the gastrodin extract.
Effect verification
The gastrodin extracts obtained in the above examples and comparative examples were subjected to HPLC detection, and the detection effects are shown in the following table:
TABLE 1 Gastrodine purity, extraction yield and time consumption for each example
| Extraction rate | Purity of | Time consuming | |
| Example 1 | 92.8％ | 98.9％ | About 2 hours |
| Example 2 | 93.7％ | 98.9％ | About 1.5 hours |
| Example 3 | 94.6％ | 99.1％ | About 3.5 hours |
| Example 4 | 95.3％ | 99.1％ | About 2 hours |
| Example 5 | 96.1％ | 99.3％ | About 4 hours |
| Comparative example 1 | 87％ | 97.1％ | About 10 hours |
| Comparative example 2 | 65％ | 97.3％ | About 24 hours |
As can be seen from table 1, the extraction rate of gastrodine in example 2 is higher than that in example 1, which may be due to the fact that complex enzyme is used for enzymolysis for a period of time in example 2, the extraction rate and purity of gastrodine in example 3 are higher than those in example 2, two stages of extraction processes should be adopted, staged extraction itself is favorable for the step-by-step extraction of active ingredients in gastrodine, and the extraction rate and purity of example 4 are both higher than those in example 3, one is the reason of staged extraction, the second is that the extraction temperature in the first stage is more favorable for the enzymolysis, and in other words, the possible enzymolysis is better in effect, so that a better extraction effect is obtained. And example 5 is a more optimized parameter in the combined use method of enzymolysis and supercritical carbon dioxide extraction, so that the best extraction effect is obtained.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the examples shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (8)
1. The gastrodin extraction process is characterized by comprising the following steps:
dissolving rhizoma gastrodiae powder in a citric acid-dipotassium hydrogen phosphate buffer solution, adjusting the pH value to 4.5-7.0, and then adding a complex enzyme accounting for 0.5-1% of the mass of the rhizoma gastrodiae powder into the buffer solution to obtain rhizoma gastrodiae powder enzymatic hydrolysate, wherein the complex enzyme comprises 2-3 parts by weight of cellulase, 1-2 parts by weight of hemicellulase, 1-3 parts by weight of papain, 1-3 parts by weight of pectinase and 1-2 parts by weight of amylase;
and step two, directly adding the rhizoma gastrodiae powder enzymolysis liquid in the step one into supercritical carbon dioxide extraction equipment for extraction, taking carbon dioxide as a solvent, taking ethanol as an entrainer, extracting at the temperature of 40-65 ℃, under the extraction pressure of 35-70 MPa for 0.5-3 hours, and finally collecting a gastrodin extract from a separation kettle of the supercritical carbon dioxide extraction equipment.
2. The gastrodin extraction process of claim 1, wherein in the first step, the gastrodin enzymolysis liquid is subjected to enzymolysis at 40-55 ℃ for 20-60 minutes under the condition of stirring, and then enters the second step.
3. The process for extracting gastrodin as claimed in claim 1, wherein in step two, CO2The flow rate is 15-30 kg/h.
4. The gastrodin extraction process of claim 1, wherein in the second step, the extraction comprises two stages, the pressure of the first stage is 35-50 Mpa, the extraction temperature is 40-55 ℃, the extraction time is 0.25-1.5 hours, the pressure of the second stage is 50-70 Mpa, the extraction temperature is 56-65 ℃, and the extraction time is 0.25-1.5 hours.
5. The gastrodin extraction process of claim 4, wherein the amount of ethanol used in the first stage is 0.2-0.5 mL, and the amount of ethanol used in the second stage is 2-3 mL.
6. The process for extracting gastrodine as claimed in claim 1, wherein the volume fraction of ethanol is 75-99%.
7. The gastrodin extraction process of claim 1, wherein in the first step, the mass volume ratio of the gastrodia elata powder to the citric acid-dipotassium hydrogen phosphate buffer solution is 1: 2-5; the pH value of the solution is adjusted by adopting HCl solution and NaOH solution.
8. The gastrodine extraction process of claim 1, wherein the particle size of the gastrodia elata powder is not larger than 100 meshes.
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Citations (5)
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|---|---|---|---|---|
| TW200520825A (en) * | 2003-12-31 | 2005-07-01 | Chi-Chun Liu | Process of extracting Gastrodiae Rhizoma by super-critical fluid |
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| CN106690173A (en) * | 2016-11-14 | 2017-05-24 | 昭通市泰旺生物科技有限公司 | Preparation method of rhizoma gastrodiae flavored potato chips |
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| TW200520825A (en) * | 2003-12-31 | 2005-07-01 | Chi-Chun Liu | Process of extracting Gastrodiae Rhizoma by super-critical fluid |
| CN101531689A (en) * | 2009-04-20 | 2009-09-16 | 陕西省科学院酶工程研究所 | Method for extracting gastrodin by biological enzyme method |
| CN102206682A (en) * | 2011-03-28 | 2011-10-05 | 南京泽朗农业发展有限公司 | Method for preparing 4-hydroxybenzyl alcohol from tall gastrodia tuber |
| CN106690173A (en) * | 2016-11-14 | 2017-05-24 | 昭通市泰旺生物科技有限公司 | Preparation method of rhizoma gastrodiae flavored potato chips |
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