CN113116948A - Method for simultaneously preparing red ginseng rhizoma phragmitis polysaccharide and extracting saponin - Google Patents
Method for simultaneously preparing red ginseng rhizoma phragmitis polysaccharide and extracting saponin Download PDFInfo
- Publication number
- CN113116948A CN113116948A CN201911391241.2A CN201911391241A CN113116948A CN 113116948 A CN113116948 A CN 113116948A CN 201911391241 A CN201911391241 A CN 201911391241A CN 113116948 A CN113116948 A CN 113116948A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- sodium hydroxide
- water
- red ginseng
- ginseng
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 235000002789 Panax ginseng Nutrition 0.000 title claims abstract description 63
- 229930182490 saponin Natural products 0.000 title claims abstract description 52
- 150000007949 saponins Chemical class 0.000 title claims abstract description 52
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 45
- 150000004676 glycans Chemical class 0.000 title claims abstract description 36
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 36
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 145
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 108
- 239000000284 extract Substances 0.000 claims abstract description 73
- 238000000605 extraction Methods 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011347 resin Substances 0.000 claims abstract description 49
- 229920005989 resin Polymers 0.000 claims abstract description 49
- 241000208340 Araliaceae Species 0.000 claims abstract description 42
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims abstract description 42
- 235000003140 Panax quinquefolius Nutrition 0.000 claims abstract description 42
- 235000008434 ginseng Nutrition 0.000 claims abstract description 42
- 239000000706 filtrate Substances 0.000 claims abstract description 36
- 238000001035 drying Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000003480 eluent Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 18
- 238000011068 loading method Methods 0.000 claims description 13
- 238000010828 elution Methods 0.000 claims description 12
- 238000010298 pulverizing process Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 7
- 238000004440 column chromatography Methods 0.000 claims description 2
- 235000017709 saponins Nutrition 0.000 description 46
- YURJSTAIMNSZAE-HHNZYBFYSA-N ginsenoside Rg1 Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YURJSTAIMNSZAE-HHNZYBFYSA-N 0.000 description 34
- FBFMBWCLBGQEBU-RXMALORBSA-N (2s,3r,4s,5s,6r)-2-[(2r,3r,4s,5s,6r)-2-[[(3s,5r,6s,8r,9r,10r,12r,13r,14r,17s)-3,12-dihydroxy-4,4,8,10,14-pentamethyl-17-[(2s)-6-methyl-2-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyhept-5-en-2-yl]-2,3,5,6,7,9,11,12,13,15,16,17-dodecah Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O FBFMBWCLBGQEBU-RXMALORBSA-N 0.000 description 32
- FBFMBWCLBGQEBU-GYMUUCMZSA-N 20-gluco-ginsenoside-Rf Natural products O([C@](CC/C=C(\C)/C)(C)[C@@H]1[C@H]2[C@H](O)C[C@H]3[C@](C)([C@]2(C)CC1)C[C@H](O[C@@H]1[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O2)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1C(C)(C)[C@@H](O)CC[C@]31C)[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 FBFMBWCLBGQEBU-GYMUUCMZSA-N 0.000 description 32
- HYPFYJBWSTXDAS-UHFFFAOYSA-N Ginsenoside Rd Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C4CCC5C(C)(C)C(CCC5(C)C4CC(O)C23C)OC6OC(CO)C(O)C(O)C6OC7OC(CO)C(O)C(O)C7O)C HYPFYJBWSTXDAS-UHFFFAOYSA-N 0.000 description 32
- UOJAEODBOCLNBU-UHFFFAOYSA-N vinaginsenoside R4 Natural products C1CC(C2(CC(O)C3C(C)(C)C(OC4C(C(O)C(O)C(CO)O4)OC4C(C(O)C(O)C(CO)O4)O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O UOJAEODBOCLNBU-UHFFFAOYSA-N 0.000 description 32
- 238000012546 transfer Methods 0.000 description 30
- 235000014676 Phragmites communis Nutrition 0.000 description 22
- 230000008569 process Effects 0.000 description 20
- 239000000843 powder Substances 0.000 description 19
- 238000012360 testing method Methods 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 14
- 229930182494 ginsenoside Natural products 0.000 description 14
- 229940089161 ginsenoside Drugs 0.000 description 14
- 239000012535 impurity Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- PWAOOJDMFUQOKB-WCZZMFLVSA-N ginsenoside Re Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](O[C@@H]2[C@H]3C(C)(C)[C@@H](O)CC[C@]3(C)[C@@H]3[C@@]([C@@]4(CC[C@@H]([C@H]4[C@H](O)C3)[C@](C)(CCC=C(C)C)O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C)(C)C2)O[C@H](CO)[C@@H](O)[C@@H]1O PWAOOJDMFUQOKB-WCZZMFLVSA-N 0.000 description 8
- AOGZLQUEBLOQCI-UHFFFAOYSA-N ginsenoside-Re Natural products CC1OC(OCC2OC(OC3CC4(C)C(CC(O)C5C(CCC45C)C(C)(CCC=C(C)C)OC6OC(CO)C(O)C(O)C6O)C7(C)CCC(O)C(C)(C)C37)C(O)C(O)C2O)C(O)C(O)C1O AOGZLQUEBLOQCI-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000011160 research Methods 0.000 description 7
- 230000033228 biological regulation Effects 0.000 description 6
- 238000001303 quality assessment method Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 230000000144 pharmacologic effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 206010028980 Neoplasm Diseases 0.000 description 2
- YURJSTAIMNSZAE-UHFFFAOYSA-N UNPD89172 Natural products C1CC(C2(CC(C3C(C)(C)C(O)CCC3(C)C2CC2O)OC3C(C(O)C(O)C(CO)O3)O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O YURJSTAIMNSZAE-UHFFFAOYSA-N 0.000 description 2
- 230000006907 apoptotic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- CBEHEBUBNAGGKC-UHFFFAOYSA-N ginsenoside Rg1 Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5CC(OC6OC(CO)C(O)C(O)C6O)C34C)C CBEHEBUBNAGGKC-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011020 pilot scale process Methods 0.000 description 2
- 239000000419 plant extract Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000013441 quality evaluation Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 206010007572 Cardiac hypertrophy Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010019799 Hepatitis viral Diseases 0.000 description 1
- 206010019851 Hepatotoxicity Diseases 0.000 description 1
- 206010035148 Plague Diseases 0.000 description 1
- 206010071362 Viral sepsis Diseases 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000006793 arrhythmia Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000005013 brain tissue Anatomy 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 230000004663 cell proliferation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000095 emetic effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 231100000304 hepatotoxicity Toxicity 0.000 description 1
- 230000007686 hepatotoxicity Effects 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000002107 myocardial effect Effects 0.000 description 1
- 208000031225 myocardial ischemia Diseases 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000004770 neurodegeneration Effects 0.000 description 1
- 208000015122 neurodegenerative disease Diseases 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 201000001862 viral hepatitis Diseases 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to an extraction method for simultaneously preparing red ginseng rhizoma phragmitis polysaccharide and saponin, which comprises the following steps: 1) crushing rhizoma Phragmitis of Ginseng radix Rubri, decocting in water, filtering decoction, and mixing filtrates; 2) feeding the filtrate into a D101 macroporous resin column, collecting the sample-feeding effluent liquid, concentrating and drying to obtain polysaccharide, wherein the sample-feeding flow rate is 1-3 BV/h; 3) the column is further washed by mixed solution of 0.3 to 3 percent of sodium hydroxide and 10 to 30 percent of ethanol with the flow rate of 1 to 3 BV/h; and then eluting with water to be colorless and neutral, eluting with 40-80% ethanol at the flow rate of 1-3 BV/h, collecting ethanol eluent, concentrating and drying to obtain the red ginseng and rhizoma phragmitis saponin extract.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, and in particular relates to a traditional Chinese medicine extraction method.
Background
The ginseng reed is the part connected with the root and stem of ginseng and is commonly called as 'reed head'. Ginseng radix Rubri is prepared by steaming Ginseng radix to destroy hydrolase and prevent hydrolysis of ginsenoside. In the process of processing ginseng into red ginseng, the corresponding ginsenoside also undergoes decarboxylation, hydrolysis and isomerization. Red ginseng is stronger than sun-dried ginseng (Sun Na, etc. the influence of the processing of ginseng on the chemical components and the pharmacological action thereof [ J ] pharmacy, 2016,27(06):857-859.) in the aspects of hepatotoxicity resistance, aging resistance, etc.
Traditionally, the rhizoma Phragmitis is considered to have emetic effect, and should be removed when in use. In industrial production, the utilization rate of the red ginseng is low, and most of the red ginseng is discarded.
Ginseng radix Rubri rhizoma Phragmitis contains effective substances such as ginsenoside and ginseng polysaccharide. Ginsenoside has the effects of treating neurodegenerative diseases in a nervous system, improving memory function, protecting brain tissues and the like, has the effects of resisting arrhythmia, myocardial hypertrophy, myocardial ischemia and myocardial apoptosis and the like in a cardiovascular system, has the effects of inducing apoptosis, inhibiting tumor cell proliferation, regulating a signal path, regulating an immune function and the like in the aspect of tumor resistance, has better clinical application value, and is applied to the treatment and prevention of various diseases (Zhuxianli, ginsenoside pharmacological action research progress [ J ]. China medicinal economy, 2017, 12(12): 152-. The pharmacological action and clinical application research of the ginseng polysaccharide are advanced, so as to provide certain guidance and reference for scientific research and high-efficiency utilization of the ginseng polysaccharide. The pharmacological actions mainly comprise anti-tumor, immunoregulation, antioxidation, anti-aging, anti-fatigue, anti-radiation, blood sugar reduction and the like; the medicine can be used for treating tumor, diabetes, viral hepatitis and sepsis (Wudawnin, etc., the pharmacological action of ginseng polysaccharide and the clinical research progress [ J ]. ginseng research, 2016, 28(05): 40-46.). How to comprehensively utilize the red ginseng rhizoma phragmitis, reduce the waste, produce high-content ginsenoside and ginseng polysaccharide, realize the resource recycling and become the difficult problem in front of people. The Chinese pharmacopoeia also only records the preparation of total saponins of ginseng stem and leaf and total saponins of ginseng, and documents (Chenyang. red ginseng compound extraction process research [ D ]. Zhejiang university, 2010.) disclose a compound extraction method of red ginseng, which comprises the steps of firstly extracting volatile oil of red ginseng by using supercritical, then extracting ginsenoside from supercritical raffinate by using ethanol as a solvent, further purifying the extract by macroporous resin to obtain a dry extract product containing ginsenoside, and finally recovering ginseng polysaccharide from red ginseng residue by using a water extraction and alcohol precipitation method. Obviously, the method for extracting red ginseng for multiple times is too complicated and is not suitable for the efficient and low-cost utilization of red ginseng rhizoma phragmitis.
In order to overcome the difficulties in the prior art, realize the recycling of traditional Chinese medicine resources and change waste into valuable, the invention researches the extraction process of the red ginseng reed head to obtain a method for industrially producing red ginseng reed head polysaccharide and saponin, and the invention also comprises the content detection of the extracted red ginseng reed head polysaccharide and saponin and the standard specification.
The invention content is as follows:
the invention provides a preparation method of a red ginseng reed head useful extract, by which the useful extract, red ginseng reed head polysaccharide and saponin can be obtained, and the method comprises the following steps:
1) crushing rhizoma Phragmitis of Ginseng radix Rubri, decocting in water, filtering decoction, and mixing filtrates;
2) feeding the filtrate into a D101 macroporous resin column, collecting the sample-feeding effluent liquid, concentrating and drying to obtain polysaccharide, wherein the sample-feeding flow rate is 1-3 BV/h;
3) the column is further washed by mixed solution of 0.3 to 3 percent of sodium hydroxide and 10 to 30 percent of ethanol with the flow rate of 1 to 3 BV/h; and then eluting with water to be colorless and neutral, eluting with 40-80% ethanol at the flow rate of 1-3 BV/h, collecting ethanol eluent, concentrating and drying to obtain the red ginseng and rhizoma phragmitis saponin extract.
Wherein,
the decocting time of the step 1) is 2-3 times, and preferably 2 times. The water addition amount for the first extraction is 5-10 times, preferably 8 times, and the water addition amount for the second extraction is 5-10 times, preferably 7 times. The extraction time is 1-3 hours, the first time is preferably 2 hours, and the second time is preferably 1.5 hours.
Wherein, the usage amount of the D101 macroporous resin column in the step 2) is the following resin weight: the weight ratio of the medicinal materials is about 0.5-1: 1, preferably 0.8: 1.
wherein, in the step 3), the ratio of the 0.3-3% sodium hydroxide solution to the 10-30% ethanol solution to the sodium hydroxide, the ethanol and the water is (0.3-3) to (7.9-23.7): (91.8-73.3); preferably 2% sodium hydroxide and 20% ethanol solution, wherein the ratio of sodium hydroxide, ethanol and water is 2.0: 15.8: 82.2, the elution amount of the sodium hydroxide and the ethanol is 4 to 9 times, preferably 6 to 7 times; the ethanol eluent has the ethanol concentration of 40-80% (v/v), preferably 60% (v/v). Washing with an ethanol solution; the elution amount is 4-9BV, preferably 5-6 BV.
Most preferably, the method of the invention comprises the following steps:
1) pulverizing rhizoma Ginseng Rubri, adding water (8 times, 7 times) and decocting for 2 times (2 hr for the first time and 1.5 hr for the second time), filtering decoction, mixing filtrates,
2) the filtrate was purified by column chromatography on D101 macroporous resin (resin weight: the weight ratio of the medicinal materials is about 0.8: 1) collecting the sample-loading effluent at a sample-loading flow rate of 1-3 BV/h, concentrating to a sugar degree of 65-85%, and drying to obtain polysaccharide;
3) ) further washing the column with 6-7BV of 2% sodium hydroxide and 20% ethanol solution at a flow rate of 1-3 BV/h; eluting with water to colorless and neutral, eluting with 5-6BV 60% ethanol at flow rate of 1-3 BV/h, collecting 60% ethanol eluate, concentrating to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), and drying to obtain Ginseng radix Rubri rhizoma Phragmitis saponin extract.
The invention is obtained by mass screening.
1. The extraction process comprises the following steps:
decocting rhizoma Phragmitis in water, filtering decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: about 0.8: 1 of medicinal materials), eluting with 0.5mol sodium hydroxide 20% ethanol, eluting with water to colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, concentrating the filtrate to fluid extract, drying, and pulverizing.
2. Experiment one: comparison experiment of different extraction times
Taking red ginseng rhizoma phragmitis (medicinal materials are not broken), adding water to extract one group for 3 times (7BV, 2 h; 6BV, 2 h; 6BV, 2h), adding water to extract the other group for 2 times (7BV, 2 h; 6BV, 1.5h), filtering decoction, combining filtrates, passing through a D101 macroporous resin column (the weight ratio of resin to medicinal materials is about 0.8: 1), eluting with water to be colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, concentrating the filtrate to be clear paste, drying and crushing to obtain the Chinese medicinal composition.
2.1 Process data statistics
2.2 statistical tables of the results of the extract tests (quality assessments)
As can be seen from the above table, compared with the process of extracting total ginsenoside for 2 times according to the 2015 edition pharmacopeia, the extraction rate of the extract is 1.8 percentage points higher, but the total saponin content is 12.1 percentage points lower, and the total amount of ginsenoside Rd + Rg1+ Re is 2.6 percentage points lower. Meanwhile, the extract prepared by extracting for 3 times is adopted, and the total saponin content and the total content of the ginsenoside Rd + Rg1+ Re do not reach the requirements; the total saponin content of the extract prepared by 2 times of extraction meets the requirement, but the total amount of the ginsenoside Rd + Rg1+ Re does not meet the requirement.
2.3 transfer Rate statistics Table for extraction Process
From the table above, it can be seen that, when the ginsenoside Re content is calculated, the extraction transfer rate is 6.1% higher and the extract transfer rate is 10.7% higher when 3 times of extraction is compared with 2 times of extraction, which indicates that the overall transfer rate is higher when 3 times of extraction is compared with 2 times of extraction, and meanwhile, when the sampling effluent, the washing solution and the elution end point sampling of 3 times and 2 times of extraction processes are detected, the ginsenoside Re content is not detected, which indicates that the effective components can be completely adsorbed by the resin dosage.
2.4 summary of experiments with different extraction times
And (3) analysis: compared with the 2-time extraction process, the 3-time extraction process has the advantages that the overall transfer rate of the finished product is high, the powder yield is also 1.8 percent, the extracted impurities are correspondingly increased, the total saponin content of the extract prepared by 3-time extraction is about 40 percent, the total content of ginsenoside Rd + Rg1+ Re is about 11 percent, and 2 indexes do not meet the target requirements of the project. The total saponin content of the extract prepared by 2 times of extraction is about 53 percent, the total content of ginsenoside Rd + Rg1+ Re is about 14 percent, and 1 index does not reach the target requirement of the project.
As a result: compared with the 2-time extraction process of the total ginsenoside according to the 2015 edition pharmacopeia, the 2-time extraction process of the extract is closer to the target of the invention, the next step is to consider the 2-time extraction process, and the quality condition of the prepared extract is inspected by comparing the crushing and non-crushing extraction of the red ginseng reed heads.
3. Experiment two: comparative experiment for crushing and non-crushing of medicinal materials
Taking the rhizoma Phragmitis of Ginseng radix Rubri, crushing one group, crushing the other group, extracting with water for 2 times (7BV, 2 h; 6BV, 1.5h), filtering the decoction, mixing the filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), eluting with water to colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, concentrating the filtrate to fluid extract, drying, and pulverizing.
3.1 Process data statistics Table
3.2 statistical Table of the results of the detection of the extracts (quality assessment)
As can be seen from the above table, by adopting the 2-time extraction process, the red ginseng reed heads are not crushed and extracted, the powder yield of the extract is low by 1.23 percent, the total saponin content is high by 7.86 percent, and the total content of the ginsenoside Rd + Rg1+ Re is high by 2.16 percent. The total saponin content of the extract prepared by extracting the reed heads for 2 times without crushing, but the total content of the ginsenoside Rd + Rg1+ Re does not reach the requirement. The total saponin content and the total amount of ginsenoside Rd + Rg1+ Re of the extract prepared by crushing the reed heads for 2 times do not reach the requirements.
3.3 transfer Rate statistics Table for extraction Process
From the above table, it can be seen that, by calculating the content of ginsenoside Re, 2 times of extraction process is adopted, the extraction transfer rate of broken red ginseng head is 8.9% higher than that of non-broken red ginseng head, the extraction transfer rate is 13.7% higher, the whole transfer rate of broken red ginseng head is higher than that of non-broken red ginseng head, and meanwhile, the ginsenoside Re content is not detected in the effluent and the washing liquid of the sample, which indicates that the extraction transfer rate is slightly better than that of non-broken red ginseng head for 2 times of breakage.
3.4 summary of the experiment of breaking and not breaking medicinal materials
And (3) analysis: by adopting the 2-time extraction process, compared with the non-crushing extraction process, the red ginseng reed head crushing process has the advantages that the integral transfer rate of the finished product after extraction is high, the powder yield is also 1.23 percent, the extracted impurities are correspondingly increased, the total saponin content of the extract prepared by the non-crushing extraction process for 2 times is about 53 percent, the total content of ginsenoside Rd + Rg1+ Re is about 14 percent, and the 1 index does not meet the target requirement of the project; the total saponin content of the extract prepared by crushing and extracting for 2 times is about 45 percent, the total content of ginsenoside Rd + Rg1+ Re is about 12 percent, and all 2 indexes do not meet the target requirements of the project.
As a result: from the results of the overall transfer rate from extraction to finished products, the extraction of the red ginseng with broken ends is higher than that of the red ginseng without breaking, and from the indexes of 2 total saponin contents of the extract and the total amount of ginsenoside Rd + Rg1+ Re, the extraction of the red ginseng with broken ends is higher than that of the red ginseng without breaking. And (5) carrying out non-crushing extraction on red ginseng reed heads, and carrying out process optimization on the resin elution process.
4. Experiment three: contrast experiment for directly collecting eluent and collecting eluent from over 10 percent of sugar degree
Taking red ginseng rhizoma Phragmitis (not broken), adding water, extracting for 2 times (7BV, 2 h; 6BV, 1.5h), filtering decoction, combining filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), eluting with water to colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, collecting one group directly, collecting the other group from eluate with sugar degree of above 10%, concentrating filtrate to fluid extract, drying, and pulverizing to obtain the final product.
4.1 Process data statistics
4.2 statistical Table of the results of the detection of the extracts (quality assessment)
As can be seen from the above table, the red ginseng reed heads are extracted by 2 times without breaking, and compared with the direct collection of the eluent which is collected from the sugar degree of more than 10%, the powder yield of the extract is lower by 0.97 percentage, the total saponin content is higher by 7.54 percentage, and the total content of the ginsenoside Rd + Rg1+ Re is higher by 1.05 percentage. The prepared extract is directly collected by eluent, the content of total saponin reaches the requirement, but the total amount of ginsenoside Rd + Rg1+ Re does not reach the requirement. The prepared extract is collected from the beginning of more than 10 percent of sugar degree, the content of the total saponin reaches about 60 percent, and simultaneously the total amount of the ginsenoside Rd + Rg1+ Re reaches the lower limit requirement.
4.3 transfer Rate statistics Table for extraction Process
From the above table, it can be seen that, by calculating the content of ginsenoside Re, the method adopts 2 times of extraction process without crushing extraction, and compared with the method of starting to collect after the sugar degree reaches more than 10%, the transfer rate of the finished product after extraction is reduced by 20.6% and 15.36% respectively by directly collecting after 60% ethanol elution, which indicates that the content transfer rate is not affected basically by discarding part of the eluent and starting to collect after the sugar degree reaches more than 10% when 60% ethanol elution is adopted.
4.4 direct collection of eluate vs. comparative experiments starting from 10% sugar
And (3) analysis: the red ginseng reed head is extracted by 2 times without breaking, eluent is directly collected and is collected from 10% of sugar degree, and compared with the direct collection of the eluent from more than 10% of sugar degree, the powder yield of the extract is low by 0.97 percentage, the content of the total saponin is high by 7.54 percentage, and the total content of the ginsenoside Rd + Rg1+ Re is high by 1.05 percentage. The prepared extract is directly collected by eluent, the content of total saponin reaches the requirement, but the total amount of ginsenoside Rd + Rg1+ Re does not reach the requirement. The prepared extract is collected from the beginning of more than 10 percent of sugar degree, the content of the total saponin reaches about 60 percent, and simultaneously the total amount of the ginsenoside Rd + Rg1+ Re reaches the lower limit requirement.
As a result: when the 60% ethanol is adopted for elution, part of eluent is discarded, and the content transfer rate is basically not influenced when the sugar degree reaches more than 10%, but the content of the total saponin is improved to a certain extent, and the yield level of the extract prepared by extracting the red ginseng without crushing the reed heads for 2 times is lower.
And the next step is to plan that after the red ginseng is crushed, the red ginseng is extracted by adding water in an amount which is twice the amount of the crushed red ginseng, so that the extraction transfer rate is improved, meanwhile, after the resin is loaded, 0.5mol of sodium hydroxide 20% ethanol is added to wash out impurities such as pigments, and whether the total saponins of the extract and the total amount of the ginsenoside Rd + Rg1+ Re can be improved or not is examined.
5. Experiment four: comparative experiment of adding 0.5mol sodium hydroxide and 20% ethanol for elution after resin sample loading
Crushing red ginseng, extracting one group with water for 2 times (8BV, 2 h; 7BV, 1.5 h; 0.8 BV, 2 h; 8BV, 1.5 h; 1.5h) and the other group with water for 2 times (10BV, 2 h; 8BV, 1.5h), filtering the decoction, merging the filtrates, passing through a D101 macroporous resin column (the weight ratio of the resin to the weight of the medicinal materials is about 0.8: 1), washing with 20% ethanol of 0.5mol of sodium hydroxide, washing with water until the filtrate is nearly neutral and colorless, eluting with 60% ethanol, collecting the eluate from the effluent with the sugar degree of more than 10%, concentrating the filtrate into clear paste, drying and crushing to obtain the red ginseng extract.
5.1 Process data statistics
5.2 statistical Table of the results of the detection of the extracts (quality assessment)
As can be seen from the above table, after the red ginseng is crushed, water (8 times, 7 times) and (10 times, 8 times) are respectively added for extraction, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added after the resin is loaded, and the powder yield of the obtained extract (8 times, 7 times) is 0.58 percentage point lower than that of the obtained extract (10 times, 8 times), the total saponin content is 3.29 percentage points, and the total content of the ginsenoside Rd + Rg1+ Re is 4.28 percentage points higher. The total saponin content and the total content of the ginsenoside Rd + Rg1+ Re all reach the requirements.
5.3 transfer Rate statistics Table for extraction Process
As can be seen from the above table, after red ginseng is crushed, water (8 times, 7 times) and water (10 times, 8 times) are respectively added for extraction, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added after resin sample loading, the extraction transfer rate (8 times, 7 times) is slightly higher than (10 times, 8 times) by 3.6 percentage points, the difference between the extraction transfer rates of finished products is small, 0.5mol of sodium hydroxide 20% ethanol is added for eluting impurities, the color of the washing liquid is obviously darker than that of washing liquid, and meanwhile, ginsenoside Rd, Rg1 and Re are not detected in the washing liquid, and no effective component is lost.
5.4 after the reed heads are broken, the water is added for extraction, and after the resin is loaded, 0.5mol of sodium hydroxide and 20 percent of ethanol are added for comparison experiment
And (3) analysis: after the red ginseng is crushed, water is added (8 times, 7 times) and (10 times, 8 times) respectively for extraction, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added after resin sample loading, the powder yield of (8 times, 7 times) extract is 0.58 percent lower than that of (10 times, 8 times), the transfer rate of the extract is not large when the extract is extracted until the finished product has a small difference, but the total saponin content is 3.29 percent, and the total content of ginsenoside Rd + Rg1+ Re is 4.28 percent higher. The total content of the total saponins of the extract and the total content of the ginsenoside Rd + Rg1+ Re all reach the requirements.
As a result: comprehensively considering the extraction transfer rate, the extract yield, the total saponin and the total amount of the ginsenoside Rd + Rg1+ Re (10 times and 8 times), the total amount of the Rd + Rg1+ Re is still low, so that the final process is determined by adding water (8 times and 7 times) to extract the crushed red ginseng reed heads respectively, and adding 0.5mol of sodium hydroxide and 20% ethanol for washing after loading the resin.
6 verification and investigation of red ginseng rhizoma phragmitis polysaccharide extract process
6.1 Process of red ginseng rhizoma phragmitis polysaccharide extract:
crushing rhizoma Ginseng Rubra, decocting in water (8 times and 7 times) for 2 times, the first 2 hr and the second 1.5 hr, filtering the decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), collecting effluent, concentrating to obtain soft extract, drying, and pulverizing.
6.2 Process data statistics
6.3 statistical Table of the results of the detection of the extracts (quality evaluation)
6.43 batches of small test experiment summary
As a result: the red ginseng is extracted by adding water (8 times and 7 times) after the red ginseng is crushed, the powder yield of 3 batches of extracts is 29.55-31.07%, the total polysaccharide content is 24.47-29.41%, the properties, the granularity and the moisture all meet the requirements, and the results of 3 batches of small experiments meet the standard requirements.
The invention has the beneficial effects that:
1. can simultaneously prepare the total ginsenoside and the ginseng polysaccharide by only one extraction;
2. by adopting the method, especially by adopting the mixed solution of sodium hydroxide and ethanol with certain concentration for elution, the content of the prepared ginseng total saponin can reach more than 55 percent, and the ginseng polysaccharide with the content of more than 20 percent is obtained at the same time.
3. The invention has simple and smooth process.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1
1. The extraction process comprises the following steps:
crushing rhizoma Ginseng Rubra, decocting in water (8 times and 7 times) for 2 times, the first 2 hr and the second 1.5 hr, filtering the decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), collecting the effluent of extractive solution sample, concentrating to soft extract, drying, and pulverizing to obtain polysaccharide extract. The column is further washed by 0.5mol sodium hydroxide 20% ethanol solution to be nearly colorless, then washed by water to be colorless and neutral, eluted by 60% ethanol, collected when the sugar degree of effluent liquid reaches more than 10%, 60% ethanol eluate is collected, filtrate is concentrated to clear paste with the relative density of 1.06-1.08(80 ℃), dried and crushed, and the ginsenoside is obtained.
1.1 Process data statistics Table
1.2 statistical Table of the results of the detection of the extracts (quality evaluation)
Total saponins of Ginseng radix
From the above table, the extraction process of adding water (8 times and 7 times) after red ginseng reed heads are crushed is adopted, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added to elute impurities after resin sample loading, the powder yield of 3 batches of extracts is between 3.1% and 3.4%, the content of total saponins is between 59.14% and 68.0%, the total content of ginsenoside Rd + Rg1+ Re is between 16.37% and 21.45%, and the content of total saponins and the total content of ginsenoside Rd + Rg1+ Re reach the requirements.
Ginseng polysaccharide
As can be seen from the above table, the process of extracting the crushed reed heads of the red ginseng by adding 8 times and 7 times of water is adopted, the decoction is carried out for 2 times, the first time is 2 hours, the second time is 1.5 hours, the decoction is filtered, the filtrates are combined, the effluent of the sample loading of the extract is collected and concentrated into thick paste by a D101 macroporous resin column (the weight ratio of the resin to the weight of the medicinal materials is about 0.8: 1), the powder yield of 3 batches of the extract is 29.55-31.07%, and the content of ginseng polysaccharide reaches the requirement of 24.47-29.41%.
1.3 transfer Rate statistics Table for extraction Process
The extraction process of crushing red ginseng reed heads and adding water (8 times and 7 times) is adopted, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added to elute impurities after resin sample loading, the extraction transfer rate is 65.37% -79.88%, the transfer rate of 60% ethanol eluent is 50.40% -52.23%, and the transfer rate of extract is 44.69% -50.45%. 0.5mol of sodium hydroxide and 20 percent of ethanol are added to elute impurities, and the effective components of the ginsenoside Rd, Rg1 and Re are not detected in washing liquor.
1.43 batches of bench test recheck test summary
And (3) analysis: the extraction process of crushing red ginseng ends and adding water (8 times and 7 times) is adopted, meanwhile, 0.5mol of sodium hydroxide 20% ethanol is added to elute impurities after resin sample loading, the powder yield of 3 batches of extracts is 3.1-3.4%, the total saponin content of 59.14-68.0% is more than 50%, the total content of ginsenoside Rd + Rg1+ Re is 16.37-21.45%, and the total content of ginsenoside Rd + Rg1+ Re is 15-25%, and the requirements are met.
As a result: the process comprises the steps of crushing red ginseng ends, adding water (8 times or 7 times) for extraction, adding 0.5mol of sodium hydroxide 20% ethanol for eluting impurities after resin sample loading, wherein the total saponin content, the total amount of ginsenoside Rd + Rg1+ Re, moisture, properties, identification, granularity, total ash content and burning residues of the extract all meet the requirements of quality standards.
Example 2
2. Process for extracting red ginseng reed head saponin
Crushing red ginseng rhizoma phragmitis, adding water (8 times and 7 times) into 120kg of the crushed red ginseng rhizoma phragmitis, decocting for 2 times, decocting for the first 2 hours and the second 1.5 hours, filtering decoction, combining filtrate, passing through a D101 macroporous resin column (the weight ratio of the resin to the medicinal materials is about 0.8: 1), firstly washing with 0.5mol of sodium hydroxide 20% ethanol solution until the filtrate is nearly colorless, then washing with water until the filtrate is colorless and neutral, eluting with 60% ethanol, collecting eluate after the sugar degree of the effluent reaches more than 10%, collecting 60% ethanol eluate, concentrating the filtrate to obtain clear paste with the relative density of 1.06-1.08(80 ℃), drying and crushing to obtain the red ginseng rhizoma phragmitis saponin.
2.1 Process data statistics
The transfer rate of the extraction in the pilot test is 81.44 percent and the average transfer rate in the minor test is 9 percent higher by calculating the content of the ginsenoside Re, which indicates that the minor test in the pilot test is fully extracted; the transfer rate of the extract in the pilot test is 42.22%, and the average transfer rate in the smaller test is 5.4% lower, which is mainly related to the higher content of the extract after resin purification, the concentration process in the pilot test and the crushing loss.
2.2 statistical tables of the results of the extract tests (quality assessments)
| Lot number and test item | Standard of merit | Pilot 20181001-1 |
| Powder yield | —— | 2.92％ |
| Moisture content | Not more than 5.0% (pharmacopeia standard) | 2.46％ |
| Total saponin content | Not less than 50% (project object) | 69.4％ |
| Rd+Rg1+Re | 15% -25% (pharmacopeia standard) | 22.1％ |
| Characteristic map | S3-S7 characteristic Peak Retention time ratio | Compliance with regulations |
| Traits | A yellow-white to gray-yellow powder; has moisture absorption | Compliance with regulations |
| Authentication | Fluorescent spots showing the same color | Identical spots |
| Particle size | The powder passing through 120 mesh sieve is not less than 95% | 96.8％ |
| Total ash content | Less than or equal to 6.0% (pharmacopeia standard) | 5.57％ |
| Residue on ignition | Less than or equal to 6.0% (pharmacopeia standard) | 2.62％ |
| Results | —— | Compliance with regulations |
The powder yield of the extract in the pilot plant test is lower by 0.35 percent, but the total saponin content is higher by 4.45 percent, and the total content of the ginsenoside Rd + Rg1+ Re is higher by 3.56 percent.
2.3 Pilot scale knots
And finally, the detection results of the total saponin content of the pilot plant extract, the total amount of the ginsenoside Rd + Rg1+ Re, the moisture, the characteristic map, the properties, the identification, the granularity, the total ash content and the ignition residues all accord with the regulations.
3. Polysaccharide extraction process
Crushing rhizoma Ginseng Rubra, decocting with water (8 times and 7 times) 120kg for 2 times, the first 2 hr and the second 1.5 hr, filtering the decoction, mixing the filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), collecting the effluent of the extractive solution, concentrating to obtain soft extract, drying, and pulverizing to obtain polysaccharide extract.
3.1 Process data statistics Table
3.2 statistical Table of the results of the detection of the extracts (quality assessment)
| Lot number and test item | Standard of merit | 20181001-2 |
| Powder yield | ≥20％ | 24.1％ |
| Moisture content | ≤10.0％ | 4.75％ |
| Total polysaccharide content | ≥15％ | 21.64％ |
| Traits | The product is light yellow to brown yellow powder; it is hygroscopic. | Compliance with regulations |
| Particle size | The powder passing through 120 mesh sieve is not less than 95% | 95.6％ |
| Results | —— | Compliance with regulations |
3.3 Pilot scale knots
And finally, the powder yield, the property, the moisture, the granularity and the polysaccharide content of the pilot plant extract all meet the requirements.
Example 4
Crushing rhizoma Ginseng Rubri, decocting with water (10 times, 5 times) 120kg for 2 times, the first 3 hr and the second 1 hr, filtering the decoction, mixing filtrates, concentrating the filtrate, and drying to obtain ginseng polysaccharide extract with polysaccharide content of 23.54%. Passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.5: 1), collecting, washing with 3% sodium hydroxide 30% ethanol solution to near colorless, washing with water to colorless, neutral, eluting with 80% ethanol, collecting eluate from effluent with sugar degree of above 10%, collecting 80% ethanol eluate, concentrating filtrate to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), drying, and pulverizing to obtain Ginseng radix Rubri rhizoma Phragmitis saponin, wherein the total ginsenoside content is 52.38%.
Example 5
Crushing rhizoma Ginseng Rubri, decocting with water (5 times ) 120kg for 2 times, the first 2 hr and the second 2 hr, filtering the decoction, mixing filtrates, concentrating the filtrate, and drying to obtain Ginseng radix polysaccharide extract with polysaccharide content of 22.18%. Passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 1: 1), collecting, washing with 0.3% sodium hydroxide 10% ethanol solution to near colorless, washing with water to colorless, neutral, eluting with 50% ethanol, collecting from effluent with sugar degree of above 10%, collecting 50% ethanol eluate, concentrating filtrate to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), drying, pulverizing to obtain Ginseng radix Rubri rhizoma Phragmitis saponin, and determining Ginseng radix total saponin 54.36%.
The content of ginsenoside is determined according to Chinese pharmacopoeia
The content determination method of ginseng polysaccharide is performed according to the marking SN/T4260-2015 of the entry and exit inspection and plague industry of the people's republic of China, the determination of crude polysaccharide in exported plant-derived food, and the phenol-sulfuric acid method.
Claims (7)
1. A method for simultaneously preparing red ginseng rhizoma phragmitis polysaccharide and saponin extraction is characterized by comprising the following steps:
1) crushing rhizoma Phragmitis of Ginseng radix Rubri, decocting in water, filtering decoction, and mixing filtrates;
2) feeding the filtrate into a D101 macroporous resin column, collecting the sample-feeding effluent liquid, concentrating and drying to obtain polysaccharide, wherein the sample-feeding flow rate is 1-3 BV/h;
3) the column is further washed by mixed solution of 0.3 to 3 percent of sodium hydroxide and 10 to 30 percent of ethanol with the flow rate of 1 to 3 BV/h; and then eluting with water to be colorless and neutral, eluting with 40-80% ethanol at the flow rate of 1-3 BV/h, collecting ethanol eluent, concentrating and drying to obtain the red ginseng and rhizoma phragmitis saponin extract.
2. The method of claim 1, wherein the number of said decocting steps of step 1) is 2-3.
3. The method according to claim 1, wherein the number of the decocting times in step 1) is 2, the amount of water added for the first time is 5-10 times, the amount of water added for the second time is 5-10 times, and the extraction time is 1-3 hours.
4. The method according to claim 1, wherein the D101 macroporous resin column in the step 2) is used in an amount of: the weight ratio of the medicinal materials is about 0.5-1: 1.
5. the method as claimed in claim 1, wherein the ratio of 0.3-3% sodium hydroxide solution and 10-30% ethanol solution in step 3) is (0.3-3) to (7.9-23.7): (91.8-73.3); the elution amount of sodium hydroxide and ethanol is 4 to 9 times; the washing elution amount of the ethanol solution is 4-9 BV.
6. The method according to claim 1, wherein the sodium hydroxide solution and the ethanol solution in step 3) are 2% sodium hydroxide and 20% ethanol solution, and the ratio of sodium hydroxide, ethanol and water is 2.0: 15.8: 82.2, the elution amount of the sodium hydroxide is 6 to 7 times of that of the ethanol.
7. The method according to claim 1, characterized in that it comprises the following steps:
1) pulverizing rhizoma Ginseng Rubra, decocting in water (8 times and 7 times) for 2 times (2 hr for the first time and 1.5 hr for the second time), filtering decoction, mixing filtrates,
2) the filtrate was purified by column chromatography on D101 macroporous resin (resin weight: the weight ratio of the medicinal materials is about 0.8: 1) collecting the sample-loading effluent at a sample-loading flow rate of 1-3 BV/h, concentrating to a sugar degree of 65-85%, and drying to obtain polysaccharide;
3) the column is further washed by 6-7BV of 2% sodium hydroxide and 20% ethanol solution, and the flow rate is 1-3 BV/h; eluting with water to colorless and neutral, eluting with 5-6BV 60% ethanol at a flow rate of 1-3 BV/h, collecting 60% ethanol eluate, concentrating to fluid extract with a relative density of 1.06-1.08 at 80 deg.C, and drying to obtain Ginseng radix Rubri rhizoma Phragmitis saponin extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911391241.2A CN113116948B (en) | 2019-12-30 | 2019-12-30 | Extraction method for simultaneously preparing polysaccharide and saponin of red ginseng and rhizoma coptidis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911391241.2A CN113116948B (en) | 2019-12-30 | 2019-12-30 | Extraction method for simultaneously preparing polysaccharide and saponin of red ginseng and rhizoma coptidis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113116948A true CN113116948A (en) | 2021-07-16 |
| CN113116948B CN113116948B (en) | 2024-03-12 |
Family
ID=76768804
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911391241.2A Active CN113116948B (en) | 2019-12-30 | 2019-12-30 | Extraction method for simultaneously preparing polysaccharide and saponin of red ginseng and rhizoma coptidis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113116948B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108338999A (en) * | 2017-01-22 | 2018-07-31 | 国药集团广东环球制药有限公司 | A kind of preparation method of sanchi leaf total saposins |
-
2019
- 2019-12-30 CN CN201911391241.2A patent/CN113116948B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108338999A (en) * | 2017-01-22 | 2018-07-31 | 国药集团广东环球制药有限公司 | A kind of preparation method of sanchi leaf total saposins |
Non-Patent Citations (3)
| Title |
|---|
| 朱梅;毕宏涛;杨威;刘杨;台桂花;周义发;: "乙醇浓度对人参多糖分离的影响", 东北师大学报(自然科学版), no. 02, pages 160 - 165 * |
| 王笳;袁崇均;陈帅;罗森;: "从西洋参中提取分离纯化人参皂苷R_(b1)和人参皂苷R_e的研究", 天然产物研究与开发, no. 02, pages 168 - 170 * |
| 诸晓波;李德坤;郭巧生;鞠爱春;叶正良;: "AB-8大孔树脂分离纯化人参保健酒皂苷的工艺研究", 中国现代中药, no. 02, pages 78 - 82 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113116948B (en) | 2024-03-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101723996B (en) | Method for separating high-purity anthocyanin monomers from black rice | |
| CN108383890B (en) | Preparation method of high-content ginsenoside Re extract | |
| CN102060891A (en) | Technological process for preparing stevioside from stevia rebaudiana bertoni | |
| CN100369648C (en) | Method for lixiviating effective components from biomass material | |
| CN112724184A (en) | Novel method for efficiently separating and preparing special compound arginine diglycoside AFG in ginseng | |
| CN102423329B (en) | A kind of discoloration method of panax notoginsenoside extract | |
| WO2020063894A1 (en) | Industrial utilization method for stevia rebaudiana and stevioside and chlorogenic acid of stevia rebaudiana | |
| CN108997469B (en) | Jujube root extract, extraction and separation method and application thereof | |
| CN112294830B (en) | American ginseng leaf product rich in rare ginsenoside | |
| CN111035666A (en) | Ginseng extract with high content of rare saponin, ginseng wine and ginseng oral liquid | |
| CN111995694B (en) | Method for decoloring and purifying polygonatum kingianum polysaccharide | |
| CN105859803B (en) | A kind of preparation method of galloyl glucose | |
| CN111297936B (en) | Method for extracting and separating total flavone, total triterpenoid saponin and total polysaccharide from momordica grosvenori roots | |
| CN106727806A (en) | A kind of preparation method of sanchi leaf total saposins | |
| Wu et al. | Efficient extraction of caffeic acid derivatives from adventitious roots of Echinacea purpurea | |
| CN108864226A (en) | A method of extracting ardisin and quercitrin from ardisia japonica | |
| CN113116948A (en) | Method for simultaneously preparing red ginseng rhizoma phragmitis polysaccharide and extracting saponin | |
| CN112315968A (en) | Ginseng leaf product rich in rare ginsenoside | |
| CN112121071A (en) | A product prepared from Ginseng radix | |
| CN107213180B (en) | Separation and extraction method of notoginseng flavone | |
| CN113116946A (en) | Method for simultaneously preparing red ginseng fibrous root polysaccharide and saponin extraction | |
| CN113429442B (en) | Method for separating tectoridin and tectorigenin from water extraction residues of rhizoma et radix Sichuan blackberry lily | |
| CN114674970A (en) | One-plate multi-information rapid thin-layer chromatography identification and inspection method for ginseng spleen-invigorating pills | |
| CN1709916A (en) | Method for extracting high purity polysaccharide of membranous milk vetch and saponin of same | |
| CN110025645B (en) | Method for extracting total saponins of American ginseng |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |