CN113116946A - Method for simultaneously preparing red ginseng fibrous root polysaccharide and saponin extraction - Google Patents
Method for simultaneously preparing red ginseng fibrous root polysaccharide and saponin extraction Download PDFInfo
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- 229930182490 saponin Natural products 0.000 title claims abstract description 42
- 150000007949 saponins Chemical class 0.000 title claims abstract description 42
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 34
- 235000002789 Panax ginseng Nutrition 0.000 title claims abstract description 31
- 150000004676 glycans Chemical class 0.000 title claims abstract description 20
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 20
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 20
- 238000000605 extraction Methods 0.000 title claims description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000284 extract Substances 0.000 claims abstract description 54
- 241000208340 Araliaceae Species 0.000 claims abstract description 32
- 235000008434 ginseng Nutrition 0.000 claims abstract description 32
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims abstract description 31
- 235000003140 Panax quinquefolius Nutrition 0.000 claims abstract description 31
- 239000000706 filtrate Substances 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 19
- 229930182494 ginsenoside Natural products 0.000 claims abstract description 16
- 229940089161 ginsenoside Drugs 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000012530 fluid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000010298 pulverizing process Methods 0.000 claims abstract description 9
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000003480 eluent Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 3
- 235000017709 saponins Nutrition 0.000 description 39
- 238000012546 transfer Methods 0.000 description 27
- 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 26
- 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 25
- 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 25
- 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 25
- 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 25
- 238000005406 washing Methods 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 5
- 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 5
- 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 5
- 238000012360 testing method Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001303 quality assessment method Methods 0.000 description 3
- 238000013441 quality evaluation Methods 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 206010027514 Metrorrhagia Diseases 0.000 description 1
- 240000004371 Panax ginseng Species 0.000 description 1
- 206010035148 Plague Diseases 0.000 description 1
- 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 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 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 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000447 pesticide residue Substances 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
- 238000003672 processing method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
Classifications
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- 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)
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- 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
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- 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
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Botany (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Sustainable Development (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Materials Engineering (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for simultaneously preparing red ginseng fibrous root polysaccharide and saponin, which comprises the following steps: 1) decocting Ginseng radix Rubri fibrous root in water, filtering decoction, and mixing filtrates; 2) loading the filtrate on D101 macroporous resin column, collecting effluent liquid, concentrating, and drying to obtain panaxan; 3) eluting the column with 80 deg.C water to colorless, eluting with ethanol solution, collecting 60% ethanol solution eluate after the sugar degree of the eluate reaches 10%, concentrating the filtrate to fluid extract, drying, and pulverizing to obtain total ginsenoside.
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
Red ginseng: is dried root and rhizome of Panax ginseng C.A.Mey. of Araliaceae. Red ginseng fibrous root: is prepared from radix Ginseng Rubra by steaming. The content of Rb1, Rb2, Rc and Rd in the fibrous root of Ginseng radix Rubri is higher than that of other parts of Ginseng radix. Red ginseng fibrous root polysaccharide: extracting Ginseng radix Rubri fibrous root, subjecting the extractive solution to resin extraction, concentrating, and drying to obtain panaxan. Red ginseng fibrous root saponin: ginseng radix Rubri fibril is extracted, resin purified, washed with water, alcohol, concentrated, and dried to obtain ginsenoside. The Ginseng radix Rubri is processed product obtained by steaming dried root and rhizome of Ginseng radix, and has effects of invigorating primordial qi, recovering pulse, relieving depletion, invigorating qi, and regulating blood. Can be used for treating asthenia, collapse, cold limbs, slight pulse, qi deficiency, blood stagnation, metrorrhagia, and metrostaxis. Red ginseng is an extremely representative important processed product of ginseng, the history of which can be traced back to the Ming Dynasty, and the earliest record on the properties of red ginseng appears in Bencao Monghuang, which refers to red ginseng with branch heads (Lu Wen Hui, et al. different steaming time has influence on ginsenoside and pesticide residue in red ginseng [ J ] Ginseng research, 2016,28(04): 2-5.). Ginseng radix Rubri is processed without whiskers (brief introduction of processing method of Ginseng radix in the introduction [ J ] and Simu Yao, 1986(03): 24-25.). The fibrous root removed from red ginseng is often treated as a waste product, and related researches show that red ginseng fibrous root also has useful value, such as related documents (Chenzhicheng, etc. the extraction process research of total ginsenosides in red ginseng fibrous root [ J ] in northwest pharmacy, 1989(02):23-25.) disclose that the total ginsenosides can be extracted from red ginseng fibrous root, namely that 85% ethanol is used for reflux extraction for 5 times, and 5 times of ethanol is used for extraction for 2 hours each time. However, the method can only extract the total saponins of ginseng at one time, and the utilization rate is low.
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 red ginseng fibrous roots to obtain an extraction method capable of industrially producing red ginseng fibrous root polysaccharide and saponin, and the invention also comprises the content detection of the extracted red ginseng fibrous root polysaccharide and saponin and the standard specification.
The invention content is as follows:
the invention provides a preparation method of a red ginseng fibrous root useful extract, by which the useful extract, red ginseng fibrous root polysaccharide and saponin can be obtained, the steps of the method are as follows:
1) decocting Ginseng radix Rubri fibrous root in water, filtering decoction, and mixing filtrates;
2) loading the filtrate on D101 macroporous resin column, collecting effluent liquid, concentrating, and drying to obtain panaxan;
3) eluting the column with water to colorless, eluting with ethanol solution, collecting ethanol solution eluate, concentrating the filtrate to fluid extract, drying, and pulverizing to obtain total ginsenoside.
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 7 times, and the water addition amount for the second extraction is 5-10 times, preferably 6 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 05-1: 1, preferably 0.8: 1.
wherein, the step 3) is eluted to be colorless by water, and the water temperature is preferably 80 ℃; washing with an ethanol solution; the elution amount is 3-7BV, preferably 4-5 BV; the ethanol concentration of the ethanol eluate is 40-80% (v/v), preferably 60% (v/v).
The preparation method of the invention, most preferably, comprises the following steps:
1) decocting Ginseng radix Rubri fibrous root in 7 times (6 times) of water for 2 times (2 hr for the first time and 1.5 hr for the second time), filtering the decoction, mixing filtrates, and passing 2) filtrate through D101 macroporous resin column (resin weight: the weight ratio of the medicinal materials is about 0.8: 1) and (3) collecting the sample-loading effluent at the sample-loading flow rate of 1-3 BV/h, concentrating and drying to obtain the ginseng polysaccharide.
3) Eluting the column with water at 80 deg.C until colorless, eluting with 4-5BV 60% ethanol, collecting 60% ethanol eluate when the sugar degree of the eluate is above 10%, concentrating the filtrate to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), and drying to obtain total ginsenoside.
The invention is obtained by mass screening, and the screening method is as follows
1. The extraction process comprises the following steps:
decocting Ginseng radix Rubri fibrous root in water, filtering decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: medicinal materials 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.
2. Experiment one: comparison experiment of different extraction times
Extracting Ginseng radix Rubri fibril, one group with water for 3 times (7BV, 2 h; 6BV, 2 h; 6BV, 2h), the other group 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.
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 2.46 percentage points higher, but the total saponin content is 14.15 percentage points lower, and the total amount of ginsenoside Rd + Rg1+ Re is 2.71 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 are all at the lower limit level; the total saponin content and the total content of ginsenoside Rd + Rg1+ Re of the extract prepared by 2 times of extraction are all in better levels.
2.3 transfer Rate statistics Table for extraction Process
As can be seen from the above table, when the ginsenoside Re content is calculated, the extraction transfer rate is 16.68% higher when 3 times of extraction is performed compared with 2 times of extraction, and the extract transfer rate is 19.19% higher, which indicates that the overall transfer rate is higher when 3 times of extraction is performed compared with 2 times of extraction, and the washing solutions of 3 times and 2 times of extraction processes and the elution end point samples of 3 times of extraction are simultaneously detected, and the ginsenoside Re content is not detected.
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 high by 2.46 percent, the total saponin content of the extract prepared by 3-time extraction is about 54.7 percent, the total content of ginsenoside Rd + Rg1+ Re is about 18.7 percent, and the overall content of the extract is at the lower limit level. The total saponin content of the extract prepared by 2 times of extraction is about 68.8 percent, the total content of ginsenoside Rd + Rg1+ Re is about 21.4 percent, and the whole content of the extract is in a better level.
As a result: compared with the process of extracting the total ginsenoside for 2 times according to the 2015 edition pharmacopeia, the total saponin content of the extract prepared by extracting for 3 times and the total content of the ginsenoside Rd + Rg1+ Re are both at the lower limit level, and the total content of the extract prepared by extracting for 2 times is at a better level. In the next step, 2 times of extraction processes are considered, impurities such as pigment and the like are removed by hot water after sample loading, meanwhile, the contrast experiment of directly collecting eluent and collecting eluent from 10% of sugar degree is considered, and the quality condition of the prepared extract is considered.
3. Experiment example two: further eluting with water of 20-80 deg.C to colorless water temperature, controlling contrast experiment, collecting Ginseng radix Rubri fibril, extracting with water for 2 times (7BV, 2 h; 6BV, 1.5h), filtering decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), eluting with water (20 deg.C), (40 deg.C), (60 deg.C) and (80 deg.C) respectively to colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, concentrating the filtrate to fluid extract, drying, and pulverizing to obtain the final product.
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, compared with the process of eluting with water at 20 deg.C, 40 deg.C, 60 deg.C and 80 deg.C to colorless, the powder yield and total saponin content of the extract are not greatly changed, the yield is reduced by 0.29%, the total saponin content is increased by 1.42%, and the total content of ginsenoside Rd + Rg1+ Re is reduced by 0.98%. But the use amount of the water washing at 80 ℃ is reduced by 1.1 times compared with that at 20 ℃, the content of the total saponin is slightly improved, and the total amount of the ginsenoside Rd + Rg1+ Re is at a middle limit level; the extract is prepared by eluting with water at 80 deg.C until colorless, and has total saponin content and total content of ginsenoside Rd + Rg1+ Re at good level.
3.3 statistical Table of transfer Rate in extraction Process (in Re)
| Batch number | 20180407-1 | 20180408-1 | 20180408-2 | 20180409-1 |
| Procedure (ii) | Transfer rate | Transfer rate | Transfer rate | Transfer rate |
| First decoction | 46.59％ | 50.32％ | 48.21％ | 51.38％ |
| Two decoctions | 27.62％ | 29.66％ | 26.55％ | 28.44％ |
| Extract liquid | 74.21％ | 79.98％ | 74.76％ | 79.82％ |
| Water washing liquid | 0 | 0 | 0 | 0 |
| Eluent | 62.86％ | 68.69％ | 65.47％ | 67.33％ |
| Transfer rate of extract | 56.80％ | 60.80％ | 59.63％ | 61.22％ |
As can be seen from the above table, when the ginsenoside Re content is calculated, compared with the process of eluting by water at 20 ℃ (40 ℃), 60 ℃ (80 ℃) and colorless, no effective component is detected in the water washing liquid, the transfer rate of the extract is not very different, which indicates that the transfer rate is not influenced by water washing at different temperatures.
3.4 column eluting with 20-80 deg.C water to colorless water temperature, and controlling contrast experiment summary
And (3) analysis: compared with the process of eluting by water at the temperature of 20 ℃, 40 ℃, 60 ℃ and 80 ℃ to be colorless, the method has the advantages that the influence on the transfer rate and the powder yield of the extract is little, the yield is reduced by 0.29 percent, the content of the total saponin is improved by 1.42 percent, and the total content of the ginsenoside Rd, Rg1 and Re is reduced by 0.98 percent.
As a result: the washing dosage of 80 ℃ is reduced by 1.1 times compared with that of 20 ℃, impurities such as pigment and the like can be better removed by adopting hot washing after sample loading, meanwhile, the content of total saponin is slightly improved, and the total amount of ginsenoside Rd + Rg1+ Re is at a middle limit level; the extract is prepared by eluting with water at 80 deg.C until colorless, and has total saponin content and total content of ginsenoside Rd + Rg1+ Re at good level.
Next examine the direct collection of the eluate versus the collection of comparative experiments starting from 2.5%, 5.0%, 7.5%, 10% sugar, examining the quality of the prepared extract.
4. Experiment three: collecting eluate directly, collecting and comparing with different sugar degrees, collecting Ginseng radix Rubri fibril, extracting with water for 2 times (7BV, 2 h; 6BV, 1.5h), filtering decoction, mixing filtrates, eluting with D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.8: 1), water-80 deg.C) to colorless, eluting with 60% ethanol, collecting 60% ethanol eluate, collecting eluate directly, collecting eluate from sugar degrees of 2.5%, 5.0%, 7.5%, and 10%, concentrating filtrate to obtain fluid extract, drying, and pulverizing.
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, compared with the comparative process of collecting the eluent from different sugar degrees of 2.5%, 5.0%, 7.5% and 10%, the powder yield of the extract has no change rule and is greatly changed, the yield difference is related to the difference of extraction transfer rate, the content of the total saponin is improved by 6.7 percentage points, and the total content of the ginsenoside Rd + Rg1+ Re is reduced by 1.16 percentage points. Directly collecting eluate and collecting eluate with different sugar degrees, wherein the content of total saponin is improved, and the total content of ginsenoside Rd + Rg1+ Re is at the middle limit level; the prepared extract is collected from the eluent with 10% of sugar degree, and the total saponin content and the total content of the ginsenoside Rd + Rg1+ Re are all in a better level.
4.3 statistical Table of transfer Rate in extraction Process (in Re)
As can be seen from the above table, when the content of the ginsenoside Re is calculated, the elution solution is directly collected, and compared with the collection process starting from 2.5%, 5.0%, 7.5% and 10% different in sugar degree, no effective component is detected in the starting receiving point, and the final transfer rate difference of the extract is mainly slightly different in the extraction process, which indicates that the collection of the elution solution from different sugar degrees has no influence on the transfer rate.
4.4 direct collection of eluent and beginning of collection of contrast experiment summary of different sugar degrees
Compared with the collection process starting from different sugar degrees of 2.5%, 5.0%, 7.5% and 10%, the direct collection of the eluent has the advantages that the different powder yield of the extract is related to the difference of extraction transfer rate, the content of the total saponin is improved, and the total content of the ginsenoside Rd + Rg1+ Re is at a middle limit level; the prepared extract is collected from the eluent with 10% of sugar degree, and the total saponin content and the total content of the ginsenoside Rd + Rg1+ Re are all in a better level.
5. And (4) conclusion: after the sample is loaded, water washing is carried out at 80 ℃, so that the water washing amount can be reduced, impurities such as pigment and the like can be removed, the influence on the transfer rate and the powder yield of the extract is small, and the content of total saponins is slightly improved; when 60% ethanol is adopted for elution, part of eluent is discarded, collection is started from the sugar degree of more than 10%, the content transfer rate is not influenced, the content of total saponin is improved to a certain extent, the yield of the extract, the total saponin and the total amount of ginsenoside Rd + Rg1+ Re are comprehensively considered, water (7 times and 6 times) is respectively added into red ginseng fibrous roots for extraction, impurities such as pigment and the like are removed by hot water washing, and meanwhile, the eluent is collected from the sugar degree of more than 10% to form the final process.
The invention has the beneficial effects that:
1. can simultaneously prepare the total ginsenoside and the ginseng polysaccharide by one-time extraction
2. The method of the invention can prepare more than 60% of total ginsenoside and 18% of ginseng polysaccharide on average.
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:
decocting Ginseng radix Rubri fibrous root in 7 times and 6 times of water 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, concentrating, and drying to obtain Ginseng radix polysaccharide; eluting with water at 80 deg.C until colorless, eluting with 60% ethanol, collecting 60% ethanol eluate when sugar degree of eluate reaches above 10%, concentrating the filtrate to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), drying, and pulverizing to obtain total ginsenoside.
2.1 statistical Table of saponin Process data
2.2 statistical Table of saponin extract test results (quality evaluation)
HPLC chart for measuring contents of 3 batches of red ginseng fibrous root ginsenoside Rd + Rg1+ Re and thin layer identification
The characteristic diagram peak measurement data table is shown by an extract detection result (quality evaluation) statistical table, the red ginseng fibrous root adopts a water (7 times and 6 times) extraction process, simultaneously, after resin sampling, water (80 ℃) is used for eluting until the red ginseng fibrous root is colorless, 60% ethanol eluent is collected after the sugar degree of the effluent reaches 10%, the powder yield of 3 batches of extracts is 4.28% -4.82%, the content of total saponins is 63.07% -76.5%, the total content of ginsenoside Rd + Rg1+ Re is 19.18% -20.72%, and the content of total saponins and the total content of ginsenoside Rd + Rg1+ Re all reach the standard requirements.
2.3 statistical Table of transfer Rate (in Re) during extraction of Saponin
| Batch number | 20180502-1 | 20180606-1 | 20180703-1 |
| Procedure (ii) | Transfer rate | ||
| First decoction | 56.47％ | 62.17％ | 41.96％ |
| Two decoctions | 26.23％ | 28.59％ | 40.70％ |
| Extract liquid | 82.70％ | 90.76％ | 82.66％ |
| 60% ethanol eluent | 76.68％ | 88.0％ | 64.21％ |
| End point of eluent | —— | —— | —— |
| Transfer rate of extract | 70.53％ | 67.26％ | 61.26％ |
The red ginseng fibrous root adopts an extraction process of adding water (7 times and 6 times), the extraction transfer rate is 82.66-90.76%, the transfer rate of 60% ethanol eluent is 64.21-88.0%, the transfer rate of extract is 61.26-67.26%, the ginsenosides Rd, Rg1 and Re are not detected at the end of elution, and the complete elution can be realized.
2.4 Experimental summary of Small trial review test of Saponin batches
And (3) analysis: the red ginseng fibrous root adopts the extraction process of adding water (7 times and 6 times), after resin sampling, water (80 ℃) is used for eluting until the red ginseng fibrous root is colorless, 60% ethanol eluent is collected from the eluent with the sugar degree of more than 10%, the powder yield of 3 batches of extracts is between 4.28% and 4.82%, the total saponin content is between 63.07% and 76.5%, the total saponin content is more than 50%, the total content of ginsenoside Rd + Rg1+ Re is 19.18% to 20.72%, the total content of ginsenoside Rd + Rg1+ Re is between 15% and 25%, and the total saponin content and the total content of ginsenoside Rd + Rg1+ Re all reach the standard requirements.
As a result: red ginseng fibrous root adopts the extraction process of adding water (7 times, 6 times), the powder yield of 3 batches of extracts is between 4.28% -4.82%, and the total saponin content of the extracts, the total amount of ginsenoside Rd + Rg1+ Re, moisture, properties, identification, granularity, characteristic spectrum, total ash content and burning residues all reach the quality standard requirements (refer to the 2015 version of Chinese pharmacopoeia for total saponin detection).
3.2 polysaccharide Process data statistics
3.3 statistical Table of polysaccharide extract test results (quality evaluation)
3.4 Experimental summary of 3 batches of polysaccharide
As a result: the extraction process of red ginseng fibrous root with 7 times and 6 times of water has 3 batches of extract with powder yield of 32.4-40.77%, total polysaccharide content of 13.83-21.07%, and properties, granularity and water content meeting the requirement, and 3 batches of bench test results meeting the standard requirement.
Example 2
Decocting Ginseng radix Rubri fibrous root with 8 times (5 times) of water for 2 times, the first 1h and the second 1h, filtering the decoction, mixing filtrates, passing through D101 macroporous resin column (resin weight: medicinal material weight ratio is about 0.5: 1), collecting the effluent of sample loading, concentrating, drying to obtain Ginseng radix polysaccharide content of 20.53%, eluting with water at 80 deg.C until colorless, eluting with 60% ethanol until sugar degree of the effluent reaches 10%, collecting 60% ethanol eluate, concentrating the filtrate to obtain fluid extract with relative density of 1.06-1.08(80 deg.C), drying, and pulverizing to obtain Ginseng radix total saponin content of 66.55%.
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 fibrous root polysaccharide and saponin extraction is characterized by comprising the following steps:
1) decocting Ginseng radix Rubri fibrous root in water, filtering decoction, and mixing filtrates;
2) loading the filtrate on D101 macroporous resin column, collecting effluent liquid, concentrating, and drying to obtain panaxan;
3) eluting the column with 80 deg.C water to colorless, eluting with ethanol solution, collecting ethanol eluate when sugar degree of the eluate reaches 10%, concentrating the filtrate to fluid extract, drying, and pulverizing to obtain total ginsenoside.
2. The method of claim 1, wherein the number of said decocting steps of step 1) is 2-3.
3. The method of claim 3, wherein the number of times of decoction in step 1) is 2; the water adding amount for the first time is 5-10 times, the water adding amount for the second time is 5-10 times, and the decocting 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 05-1: 1.
5. the method of claim 1, wherein step 3) a ethanol wash; the elution amount is 3-7 BV; the ethanol concentration of the ethanol eluent is 40-80% v/v.
6. The method of claim 1, wherein step 3) a ethanol wash; the elution amount is 4-5 BV; the ethanol concentration of the ethanol eluate was 60% v/v.
7. The method according to claim 1, characterized in that it comprises the following steps:
1) decocting Ginseng radix Rubri fibrous root with 7 times and 6 times of water for 2 times, the first 2 hr and the second 1.5 hr, filtering decoction, and mixing filtrates;
2) the filtrate is passed through a D101 macroporous resin column, and the weight of the resin is as follows: the weight ratio of the medicinal materials is about 0.8: 1, sampling at the flow speed of 1-3 BV/h, collecting the sample effluent, concentrating and drying to obtain the ginseng polysaccharide;
3) eluting the column with 80 deg.C water to colorless, eluting with 4-5BV 60% ethanol, collecting 60% ethanol eluate when the sugar degree of the eluate is above 10%, concentrating the filtrate to fluid extract with relative density of 1.06-1.08 at 80 deg.C, and drying to obtain total ginsenoside.
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