CN107141326B - Method for extracting baicalin from scutellaria baicalensis - Google Patents
Method for extracting baicalin from scutellaria baicalensis Download PDFInfo
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- CN107141326B CN107141326B CN201710449407.6A CN201710449407A CN107141326B CN 107141326 B CN107141326 B CN 107141326B CN 201710449407 A CN201710449407 A CN 201710449407A CN 107141326 B CN107141326 B CN 107141326B
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- baicalin
- radix scutellariae
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- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 title claims abstract description 23
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 title claims abstract description 23
- 229960003321 baicalin Drugs 0.000 title claims abstract description 23
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 14
- 240000004534 Scutellaria baicalensis Species 0.000 title claims abstract description 10
- 235000017089 Scutellaria baicalensis Nutrition 0.000 title claims abstract description 10
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000012510 hollow fiber Substances 0.000 claims abstract description 9
- 102000004190 Enzymes Human genes 0.000 claims abstract description 7
- 108090000790 Enzymes Proteins 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 13
- 239000004382 Amylase Substances 0.000 claims description 8
- 102000013142 Amylases Human genes 0.000 claims description 8
- 108010065511 Amylases Proteins 0.000 claims description 8
- 108090000145 Bacillolysin Proteins 0.000 claims description 8
- 102000035092 Neutral proteases Human genes 0.000 claims description 8
- 108091005507 Neutral proteases Proteins 0.000 claims description 8
- 235000019418 amylase Nutrition 0.000 claims description 8
- 230000002255 enzymatic effect Effects 0.000 claims description 8
- 239000000413 hydrolysate Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 108010059892 Cellulase Proteins 0.000 claims description 6
- 229940106157 cellulase Drugs 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 229940088598 enzyme Drugs 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 abstract description 9
- 238000009776 industrial production Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- 241000207929 Scutellaria Species 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 206010000234 Abortion spontaneous Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000941 bile Anatomy 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000027939 micturition Effects 0.000 description 1
- 208000015994 miscarriage Diseases 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 210000002460 smooth muscle Anatomy 0.000 description 1
- 208000000995 spontaneous abortion Diseases 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- 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
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- 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)
- Medicines Containing Plant Substances (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a method for extracting baicalin from scutellaria baicalensis, which is prepared by carrying out enzymolysis through three enzymes, then sending the three enzymes into a hollow fiber membrane cylinder, and separating and purifying by adopting a membrane separation technology. The invention can be completed by only two steps, simplifies the working procedures, reduces the cost (saves about 62 percent of the cost), is more suitable for industrial production, improves the quality of the baicalin, improves the extraction rate, and ensures that the content of the finished product can reach more than 98 percent.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, and particularly relates to a method for extracting baicalin from scutellaria baicalensis.
Background
The scutellaria is a common traditional Chinese medicine, has the efficacies of clearing away heat and toxic material, purging fire for removing toxin, stopping bleeding, preventing miscarriage and the like, has wide clinical application and does not generate drug resistance. Baicalin is one of the important active ingredients of radix Scutellariae, and has pharmacological proven effects of inhibiting bacteria, clearing heat, lowering blood pressure, promoting urination, protecting liver, promoting bile flow, tranquilizing mind, relieving smooth muscle spasm, resisting allergy, inflammation and cancer. Baicalin can absorb ultraviolet rays, remove oxygen free radicals, and inhibit melanin generation, so it can be used in medicine and cosmetics.
The traditional extraction method of baicalin is to cut fresh baical skullcap root, heat and boil with 10 times of water for extraction, combine the extract, place the extract to normal temperature, add acid to adjust pH value, then the baicalin settles to the bottom, remove the supernatant, add water to the precipitate and stir, continue to adjust acid to obtain the crude baicalin precipitate, then crystallize and recrystallize with proper solvent to obtain the product. The method has the defects of long extraction time, high cost, low extraction rate and the like.
CN 103044507B discloses a process for extracting baicalin from wild scutellaria baicalensis, which comprises the steps of enzymolysis with compound cellulase, ultrasonic ethanol extraction, filtration, primary refining of polyamide, ethanol elution, recrystallization, etc., and is said to obtain baicalin with purity of more than 98%. But the process is complex, the production period is long, and the production cost is high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a novel method for extracting baicalin from scutellaria baicalensis, which can be completed by only two steps and is more suitable for industrial production.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for extracting baicalin from scutellaria baicalensis is completed by the following steps:
(1) enzymolysis: pulverizing radix Scutellariae to 40-60 mesh, adding appropriate amount of water and enzyme, hydrolyzing with cellulase, amylase and neutral protease at an appropriate temperature of 40 deg.C, pH of 4.5-6.5, activity of 10 ten thousand units per gram, and action time of 1-1.5 hr; the addition amount of amylase is 0.5-1.0% of the substrate, the appropriate temperature is 50-55 ℃, the pH value is 6.8, the activity is 5000 units per gram, and the action time is 0.5-1 h; the addition amount of the neutral protease is 0.05-0.25%, the appropriate temperature is 35-55 ℃, the pH value is 6.5-7.2, the activity is 10 ten thousand units per gram, and the action time is 0.5-0.8 h; then adjusting pH to 3-5, heating to boil, maintaining boiling state for 1-2 hr, and separating to obtain Scutellariae radix residue and enzymolysis solution;
(2) membrane separation: and (3) cooling the enzymatic hydrolysate obtained in the step (2) to normal temperature, then sending the enzymatic hydrolysate into a hollow fiber membrane cylinder, and separating and purifying by adopting a membrane separation technology to obtain the baicalin product.
Preferably, in the enzymolysis step, weakly alkaline small molecular group water is added into the filtered radix scutellariae residue, 6-10 liters of weakly alkaline small molecular group water is added into each kilogram of radix scutellariae residue, the radix scutellariae residue and the extracting solution are extracted for 2-4 hours at the temperature of 20-25 ℃, and the radix scutellariae residue and the extracting solution are separated again, wherein the extracting solution and the enzymolysis solution are sent into a hollow fiber membrane cylinder for separation and purification.
Compared with the prior art, the invention has the beneficial effects that: 1. the whole extraction process can be completed by only two steps, so that the process is simplified, the cost is reduced (about 62 percent of cost is saved), and the method is more suitable for industrial production; 2. three kinds of enzymolysis and heating boiling are adopted, so that the release rate of the baicalin from the scutellaria baicalensis is accelerated, the use of a solvent ethanol and the damage of acid and alkali on the baicalin are avoided, and the quality and the extraction rate of the baicalin are improved; 3. the membrane separation technology is adopted to complete the functions of separation, purification, refining and the like at one time, the extraction time is saved, and the content of the finished product can reach more than 98 percent.
Detailed Description
The present invention will now be described in further detail with reference to specific embodiments. It is clear that the invention is not thus limited to the scope of the embodiments described. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of the present invention. The experimental methods in the following examples, which are not specified under specific conditions, were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example one
The method for extracting baicalin from scutellaria baicalensis is completed by the following steps:
(1) enzymolysis: pulverizing radix Scutellariae to 60 mesh, adding appropriate amount of water, adding enzyme, and hydrolyzing, wherein the enzyme is cellulase, amylase and neutral protease, the cellulase is added in an amount of 2% of the substrate, the appropriate temperature is 40 deg.C, pH is 5.5, activity is 10 ten thousand units per gram, and the action time is 1 h; the addition amount of amylase is 0.5 percent of the substrate, the appropriate temperature is 50 ℃, the pH value is 6.8, the activity is 5000 units per gram, and the action time is 0.5 h; the addition amount of the neutral protease is 0.05 percent, the appropriate temperature is 35 ℃, the pH value is 6.5, the activity is 10 ten thousand units per gram, and the action time is 0.5 h; then adjusting pH to 5, heating and boiling, maintaining boiling state for 2 hr, and separating to obtain Scutellariae radix residue and enzymolysis solution;
(2) membrane separation: and (3) cooling the enzymatic hydrolysate obtained in the step (2) to normal temperature, then sending the enzymatic hydrolysate into a hollow fiber membrane cylinder, and separating and purifying by adopting a membrane separation technology to obtain the baicalin product.
In the enzymolysis step, weakly alkaline small molecular group water is added into the filtered radix scutellariae residue, 6 liters of weakly alkaline small molecular group water is added into each kilogram of radix scutellariae residue, the radix scutellariae residue and the extracting solution are separated again at 25 ℃ and are sent into a hollow fiber membrane cylinder together with the enzymolysis solution for separation and purification.
Example two
Pulverizing radix Scutellariae to 40 mesh, adding appropriate amount of water and enzyme, hydrolyzing with cellulase, amylase and neutral protease at an appropriate temperature of 40 deg.C, pH of 6.5, activity of 10 ten thousand units per gram, and action time of 1.5 hr; the addition amount of amylase is 1.0 percent of the substrate, the appropriate temperature is 55 ℃, the pH value is 6.8, the activity is 5000 units per gram, and the action time is 1 h; the addition amount of the neutral protease is 0.25 percent, the proper temperature is 55 ℃, the pH value is 7.2, the activity is 10 ten thousand units per gram, and the action time is 0.8 h; then adjusting pH to 4, heating and boiling, maintaining boiling state for 1h, and separating to obtain Scutellariae radix residue and enzymolysis solution;
(2) membrane separation: and (3) cooling the enzymatic hydrolysate obtained in the step (2) to normal temperature, then sending the enzymatic hydrolysate into a hollow fiber membrane cylinder, and separating and purifying by adopting a membrane separation technology to obtain the baicalin product.
In the enzymolysis step, weakly alkaline small molecular group water is added into the filtered radix scutellariae residue, 10 liters of weakly alkaline small molecular group water is added into each kilogram of radix scutellariae residue, the radix scutellariae residue and the extracting solution are separated again at the temperature of 20 ℃ and are sent into a hollow fiber membrane cylinder together with the enzymolysis solution for separation and purification.
Claims (1)
1. A method for extracting baicalin from scutellaria baicalensis is completed by the following steps:
(1) enzymolysis: pulverizing radix Scutellariae to 40-60 mesh, adding appropriate amount of water and enzyme, hydrolyzing with cellulase, amylase and neutral protease at an appropriate temperature of 40 deg.C, pH of 4.5-6.5, activity of 10 ten thousand units per gram, and action time of 1-1.5 hr; the addition amount of amylase is 0.5-1.0% of the substrate, the appropriate temperature is 50-55 ℃, the pH value is 6.8, the activity is 5000 units per gram, and the action time is 0.5-1 h; the addition amount of the neutral protease is 0.05-0.25%, the appropriate temperature is 35-55 ℃, the pH value is 6.5-7.2, the activity is 10 ten thousand units per gram, and the action time is 0.5-0.8 h; then adjusting pH to 3-5, heating to boil, maintaining boiling state for 1-2 hr, and separating to obtain Scutellariae radix residue and enzymolysis solution; adding weakly alkaline small molecular group water into the filtered radix Scutellariae residue, adding 6-10L weakly alkaline small molecular group water into each kilogram of radix Scutellariae residue, extracting at 20-25 deg.C for 2-4h, separating radix Scutellariae residue and extractive solution, wherein the extractive solution and enzymolysis solution are fed into hollow fiber membrane column for separation and purification;
(2) membrane separation: and (3) cooling the enzymatic hydrolysate obtained in the step (2) to normal temperature, then sending the enzymatic hydrolysate into a hollow fiber membrane cylinder, and separating and purifying by adopting a membrane separation technology to obtain the baicalin product.
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| CN109867706A (en) * | 2019-04-04 | 2019-06-11 | 楚雄医药高等专科学校 | The method for extraction and purification of effective component in a kind of Yi nationality's medicine fleabane flower |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182247A (en) * | 2012-12-18 | 2013-07-03 | 神威药业集团有限公司 | Method for improving safety of traditional Chinese medicine injection |
| CN104784254A (en) * | 2015-04-03 | 2015-07-22 | 宝鸡市虹源生物科技有限公司 | Extraction method for producing baicalin with biological enzyme method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182247A (en) * | 2012-12-18 | 2013-07-03 | 神威药业集团有限公司 | Method for improving safety of traditional Chinese medicine injection |
| CN104784254A (en) * | 2015-04-03 | 2015-07-22 | 宝鸡市虹源生物科技有限公司 | Extraction method for producing baicalin with biological enzyme method |
Non-Patent Citations (1)
| Title |
|---|
| 应用膜技术浓缩黄芩苷提取液的研究;周显宏等;《东莞理工学院院报》;20080228;第15卷(第1期);46-51 * |
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