CN106727806A - A kind of preparation method of sanchi leaf total saposins - Google Patents
A kind of preparation method of sanchi leaf total saposins Download PDFInfo
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- CN106727806A CN106727806A CN201611196949.9A CN201611196949A CN106727806A CN 106727806 A CN106727806 A CN 106727806A CN 201611196949 A CN201611196949 A CN 201611196949A CN 106727806 A CN106727806 A CN 106727806A
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- ethanol
- sanchi leaf
- preparation
- total saposins
- leaf total
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- 239000009759 San-Chi Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 229930182494 ginsenoside Natural products 0.000 claims abstract description 26
- 229940089161 ginsenoside Drugs 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000008280 blood Substances 0.000 claims abstract description 9
- 210000004369 blood Anatomy 0.000 claims abstract description 9
- 208000002193 Pain Diseases 0.000 claims abstract description 6
- 239000003814 drug Substances 0.000 claims abstract description 5
- 230000007812 deficiency Effects 0.000 claims abstract description 4
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 claims abstract description 3
- 206010022437 insomnia Diseases 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 160
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000011347 resin Substances 0.000 claims description 32
- 229920005989 resin Polymers 0.000 claims description 31
- 238000010828 elution Methods 0.000 claims description 25
- 239000000284 extract Substances 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 11
- 239000012467 final product Substances 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 239000013558 reference substance Substances 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 244000131316 Panax pseudoginseng Species 0.000 claims description 4
- 235000003181 Panax pseudoginseng Nutrition 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 abstract description 9
- 229930182490 saponin Natural products 0.000 abstract description 9
- 150000007949 saponins Chemical class 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
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- 206010054949 Metaplasia Diseases 0.000 abstract 1
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- 239000002552 dosage form Substances 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 230000015689 metaplastic ossification Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
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- 238000001179 sorption measurement Methods 0.000 description 8
- 238000003795 desorption Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
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- 241000180649 Panax notoginseng Species 0.000 description 3
- 235000003143 Panax notoginseng Nutrition 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000001814 pectin Substances 0.000 description 3
- 235000010987 pectin Nutrition 0.000 description 3
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- 150000001720 carbohydrates Chemical class 0.000 description 2
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- 239000000049 pigment Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HERICYNRBVMDFO-WVYXDZFESA-N (2r,3r,4s,5s,6r)-2-[[(2r,3s,4s,5r,6s)-6-[(2s)-2-[(3s,5r,8r,9r,10r,12r,13r,14r,17s)-3-[(2r,3r,4s,5s,6r)-3-[(2s,3r,4s,5s,6r)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2s,3r,4s,5r)-3,4,5-trihydroxyoxan-2-yl]oxyoxan-2-yl]oxy-4,5-dihydroxy-6-(hydroxymethyl)oxan-2-yl Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)CO5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HERICYNRBVMDFO-WVYXDZFESA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 208000034656 Contusions Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000208343 Panax Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 208000034526 bruise Diseases 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
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- 230000000295 complement effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- -1 filter Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- NODILNFGTFIURN-USYOXQFSSA-N ginsenoside Rb3 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1OC[C@@H](O)[C@H](O)[C@H]1O NODILNFGTFIURN-USYOXQFSSA-N 0.000 description 1
- 229930187479 gypenoside Natural products 0.000 description 1
- ZRBFCAALKKNCJG-UHFFFAOYSA-N gypenoside-XVII Natural products C1CC(C2(CCC3C(C)(C)C(OC4C(C(O)C(O)C(CO)O4)O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC(C(C(O)C1O)O)OC1COC1OC(CO)C(O)C(O)C1O ZRBFCAALKKNCJG-UHFFFAOYSA-N 0.000 description 1
- 208000035861 hematochezia Diseases 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- PWVJRANWWJJIOF-QVAFKJSISA-N notoginsenoside Fa Natural products CC(=CCC[C@](C)(O[C@@H]1O[C@H](CO[C@@H]2O[C@H](CO)[C@@H](O)[C@H](O)[C@H]2O)[C@@H](O)[C@H](O)[C@H]1O)[C@H]3CC[C@]4(C)[C@@H]3[C@H](O)C[C@@H]5[C@@]6(C)CC[C@H](O[C@@H]7O[C@H](CO)[C@@H](O)[C@H](O)[C@H]7O[C@@H]8O[C@H](CO)[C@@H](O)[C@H](O)[C@H]8O[C@H]9[C@H](O)OC[C@@H](O)[C@@H]9O)C(C)(C)[C@@H]6CC[C@@]45C)C PWVJRANWWJJIOF-QVAFKJSISA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 206010033675 panniculitis Diseases 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 210000004304 subcutaneous tissue Anatomy 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 230000008736 traumatic injury Effects 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)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- 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
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- 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)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Physics & Mathematics (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to effective ingredients in plant beneficiation technologies field, a kind of preparation method of the raw material sanchi leaf total saposins of preparation (Qiyeshen' and tablet) is specifically disclosed, the method is with ginsenoside Rb3Content is the sanchi leaf total saposins preparation method that evaluation index is set up.Qiyeshen' and tablet has benefiting qi for tranquillization, promoting blood circulation and stopping pain effect, it is palpitaition, insomnia caused by for treating deficiency of heart-QI, the stagnation of the heart blood, chest pain, uncomfortable in chest, its prescription raw material is the sanchi leaf total saposins of gained after the extracted separation of sanchi leaf is decolourized, and preparation method disclosed by the invention is with ginsenoside Rb3Content sets up sanchi leaf total saposins preparation method for evaluation index.Sanchi leaf total saponin content that the preparation method is obtained is high, produce feasible, process stabilizing, improves the quality controllability of sanchi leaf total saposins, so as to ensure the quality and validity of its finished dosage form Qiyeshen' and tablet, is easy to drug standards metaplasia to produce.
Description
Technical field
The invention belongs to effective ingredients in plant beneficiation technologies field, a kind of preparation (Qiyeshen' and tablet) is specifically disclosed
Raw material sanchi leaf total saposins preparation method, the method is with ginsenoside Rb3Content is the sanchi leaf that evaluation index is set up
Total saposins preparation method, obtained sanchi leaf total saposins are used to prepare palpitaition, the mistake caused by treatment deficiency of heart-QI, the stagnation of the heart blood
Sleep, chest aches, Chinese medicine preparation Qiyeshen' and tablet uncomfortable in chest.
Background technology
Sanchi leaf is the leaf of panax araliaceae plant Panax notoginseng (Burk.) F.H.Chen, is stopped with the scattered stasis of blood
The effect of blood, detumescence ding-tong, it is usually used in spitting blood, bleeding from five sense organs or subcutaneous tissue is had blood in stool, traumatism and bleeding, treating swelling and pain by traumatic injury, carbuncle sore tumefacting virus.《Compendium of Materia Medica》
Claim notoginseng haulm " control injured, fall and put out blood, that applies stops, and bruise is to dissipate through night, the same root of complementary work ".Studied through modern chemical analysis
Main component is ginsenoside Rb in proving sanchi leaf1, ginsenoside Rb3, Re, gypenoside and notoginsenoside Fa, Fc, Fe
Deng.Modern pharmacological research show sanchi leaf total saposins have reducing blood lipid, tranquilizing and allaying excitement, improve experimental animal body's immunity and
The effect such as extension life-span；There is obvious analgesic activity to the pain that thermostimulation and chemical stimulation cause, its analgesic activity is
By improving the threshold of pain, suppress central and the periphery property induced pain factor and produce, onset of action is fast, length of holding time；To the cerebrovascular
There is contraction, and inhibitory action is presented to platelet aggregation.
Existing process：Sanchi leaf decocting is boiled, and concentrate is concentrated into right amount, plus ethanol makes alcohol content up to 60%, standing make to sink
Form sediment, take supernatant, filter, activated carbon decolorizing, destainer reclaims ethanol and is concentrated into right amount, dries, and obtains final product.
The present invention is mainly improved relative to existing process at following aspects：1. boiled because of decocting and easily decocted out largely
Impurity, particularly sugar and pectin constituents, the present invention extract solvent by investigating, and increased 70% ethanol is carried out to sanchi leaf
Extract, the ginsenoside Rb that 70% ethanol is extracted3The rate of transform far above water extract.2. decoloration process by existing process activity
Charcoal or organic reagent extraction are improved to the decolouring of D101 macroreticular resins, compared with the prior art, also can outside removal fat-soluble pigment
Water colo(u)r is removed, and part carbohydrate and pectin can be removed while decolourizing, saponin content in lifting sanchi leaf total saposins.
3. sanchi leaf total saponin content and producing feasibility have been taken into account, has been easy to industrialization.
Total saposins composition in thering are Part Methods to be enriched with sanchi leaf in prior art research, obtained sanchi leaf total saposins
With ginsenoside Rb3Be index meter total saponin content major part below 10%, have the made content of portion of techniques slightly higher but cannot
Adapt to big production needs.Separately due to containing a large amount of pigments, carbohydrate and pectin in saponin of Radix Notoginseng leaf, using traditional in enrichment process
It is undesirable that organic solvent, activated carbon, aluminum oxide etc. carry out removal of impurities decolouring.We are by using the side for extracting plus alcohol precipitation/water sinks
Formula, in conjunction with macroporous absorbent resin decolouring removal of impurities, multiple batches of obtained sanchi leaf total saposins are with ginsenoside Rb3For index meter is total
Saponin content is above more than 10%, and has passed through corresponding production checking, realizes large-scale production, and stable preparation process can
OK, so as to ensure that the quality stability of Qiyeshen' and tablet different batches of product.
The content of the invention
It is an object of the invention to provide the preparation method of sanchi leaf total saposins.
Sanchi leaf total saposins of the present invention are the primary raw materials of Chinese medicine preparation Qiyeshen' and tablet.
The preparation method of sanchi leaf total saposins of the present invention, the method is with ginsenoside Rb3Content refers to for evaluation
The sanchi leaf total saposins preparation method set up is marked, is comprised the following steps：
1) solvent extraction will be used after sanchi leaf coarse crushing, obtain pseudo-ginseng leaf extract, the solvent will be selected from water, 70% ethanol and appoints
Meaning is a kind of；
2) after gained pseudo-ginseng leaf extract inspissated juice relative density is 1.10~1.25 (60 DEG C), ethanol is added to make alcohol content
Enter water-filling and sink to 50%~70% or 3~7 times of amount water of addition, standing separation takes supernatant；
3) supernatant is decolourized by macroreticular resin, is first eluted with water and low-concentration ethanol, and 70% ethanol elution is used afterwards,
Eluent is collected, ethanol is reclaimed, concentrate drying is obtained final product.
Wherein, step 2) described in extract concentration be concentrated into relative density for 1.15~1.20 (60 DEG C)；
Wherein, step 2) described in ethanol final concentration of 55%~65%；
Wherein, step 2) described in water addition for 5~6 times amount；
Wherein, step 3) described in macroreticular resin be D101 macroreticular resins；
Wherein, step 3) described in washing consumption be 3~6BV consumptions；
Wherein, step 3) described in low-concentration ethanol be 20%~30% ethanol；
Wherein, step 3) described in low-concentration ethanol consumption be 3~6BV (column volume) consumption；
Wherein, step 3) described in 70% ethanol consumption be 4~6BV (column volume) consumption；
Preferably, the preparation method of sanchi leaf total saposins of the present invention, comprises the following steps：
Sanchi leaf 1kg is taken, plus 10-20 times is measured 50-90% alcohol refluxs and extracted 1-3 times, each 2-4h, extract solution filtering,
Merge, concentration, plus 4-6 times measured water and enter water-filling and sink, and is stood, filtering, and filtrate concentration, upper D101 macroreticular resins decolourize, with 6BV water and
The ethanol elution removal of impurities of 4BV 25%, finally with the ethanol elutions of 5BV 70%, collects 70% ethanol eluate, and concentration is dried, obtained
To sanchi leaf total saposins.
Or,
Sanchi leaf 1kg is taken, plus 10-20 times is measured water refluxing extraction 1-3 times, each 2-4h, extract solution merges concentration, plus ethanol
Make alcohol content up to 50-70%, stand, filtering, filtrate concentration, upper D101 macroreticular resins decolourize, successively with 6BV water, 4BV 30%
Ethanol and the ethanol elutions of 5BV 70%, collect 70% ethanol eluate, and concentration is dried, and obtains sanchi leaf total saposins.
It is further preferred that the preparation method of sanchi leaf total saposins of the present invention, comprises the following steps：
Sanchi leaf 1kg is taken, plus 15 times of 70% alcohol refluxs of amount are extracted 2 times, each 3h, extract solution is filtered, merges, is concentrated into
Relative density 1.20, plus 5 times of amount water enter water-filling and sink, and after standing 24h, filtering, filtrate is concentrated into 1.07~1.09, upper D101 macropores
Resin decolorization, blade diameter length ratio 1：8~1：10, with the ethanol elution removal of impurities of 6BV water and 4BV 25%, finally washed with the ethanol of 5BV 70%
It is de-, 70% ethanol eluate is collected, concentration is dried, and obtains sanchi leaf total saposins.
Or,
Sanchi leaf 1kg is taken, plus 15 times are measured water refluxing extraction 2 times, each 3h, extract solution merging is concentrated into relative density
1.20, plus ethanol makes alcohol content up to 60%, after standing 24h, filtering, filtrate is concentrated into 1.07~1.09, upper D101 macroreticular resins
Decolourize, blade diameter length ratio 1：8~1：10, loading flow velocity is 1BV/h, is successively washed with 6BV water, the ethanol of 4BV 30%, the ethanol of 5BV 70%
It is de-, 70% ethanol eluate is collected, concentration is dried, and obtains sanchi leaf total saposins.
Wherein, 6BV refers to D101 macroreticular resins column volume used by 6 times；
Wherein, 5BV refers to D101 macroreticular resins column volume used by 5 times；
Wherein, 4BV refers to D101 macroreticular resins column volume used by 4 times；
It is another object of the present invention to provide sanchi leaf total saposins in treatment deficiency of heart-QI, caused by the stagnation of the heart blood
Applied in palpitaition, insomnia, chest pain, Chinese medicine preparation Qiyeshen' and tablet uncomfortable in chest.
It is another object of the present invention to provide sanchi leaf total saposins (with ginsenoside Rb3Be index meter) measure side
Method.
Assay method of the present invention, comprises the following steps：
Determined according to high performance liquid chromatography (four general rules 0512 of Chinese Pharmacopoeia version in 2015).
Chromatographic condition is tested with octadecylsilane chemically bonded silica as filler with system suitability；It is flowing with acetonitrile
Phase A, is Mobile phase B with 0.2% phosphoric acid solution, and the regulation according to the form below carries out gradient elution；Detection wavelength is 203nm.It is theoretical
The number of plates presses ginsenoside Rb3Peak is calculated and should be not less than 6000.
The preparation of reference substance solution takes ginsenoside Rb3Appropriate reference substance, it is accurately weighed, plus ethanol is made every 1ml and contains
The solution of 0.5mg, obtains final product.
The preparation of need testing solution takes sanchi leaf total saposins 50mg, accurately weighed, puts in 10ml measuring bottles, is dissolved with ethanol
And scale is diluted to, and shake up, filter, subsequent filtrate is taken, obtain final product.
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines,
Obtain final product.
Sanchi leaf total saposins preparation method disclosed by the invention, the method is by improving on the basis of existing method
Arrive, by way of heavy using extraction plus alcohol precipitation/water, in conjunction with macroporous absorbent resin decolouring removal of impurities, multiple batches of obtained three
Seven leaf total saposins are with ginsenoside Rb3For index meter total saponin content is above more than 10%, and corresponding production is passed through and has tested
Card, realizes large-scale production, and stable preparation process is feasible, so as to ensure that its formulation products Qiyeshen' and tablet different batches is produced
The quality stability of product.Simultaneously as sanchi leaf total saposins are the main actives of Qiyeshen' and tablet, the present invention is improving three
While seven leaf total saposins quality, the curative effect of Qiyeshen' and tablet is also improved.
Brief description of the drawings
Fig. 1 is sanchi leaf total saposins preparation technology flow chart,
Fig. 2 is Different solution elution curve when D101 macroreticular resins are eluted.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply the content described by example and be merely to illustrate the present invention, without should also without limitation on sheet described in detail in claims
Invention.
The preparation of the sanchi leaf total saposins of embodiment 1
Sanchi leaf 1kg is taken, plus 15 times of 70% alcohol refluxs of amount are extracted 2 times, each 3h, extract solution is filtered, merges, is concentrated into
Relative density 1.20 (60 DEG C), plus 5 times of amount water enter water-filling and sink, and after standing 24h, filtering, filtrate is concentrated into 1.07~1.09 (60
DEG C), upper D101 macroreticular resins decolourize, blade diameter length ratio 1：8~1：10, loading flow velocity is 1BV/h, with 6BV water (elution speed 3BV/h)
With the ethanol elution removal of impurities of 4BV 25%, finally eluted with the ethanol (elution speed 2BV/h) of 5BV 70%, collect 70% ethanol and wash
De- liquid, concentration is dried, and obtains sanchi leaf total saposins 65.7g, and high performance liquid chromatography measures ginsenoside Rb3Content is
12.99%.
The preparation of the sanchi leaf total saposins of embodiment 2
Sanchi leaf 1kg is taken, plus 15 times are measured water refluxing extraction 2 times, each 3h, extract solution merging is concentrated into relative density 1.20
(60 DEG C), plus ethanol makes alcohol content up to 60%, and after standing 24h, filtering, filtrate is concentrated into 1.07~1.09 (60 DEG C), upper D101
Macroreticular resin decolourizes, blade diameter length ratio 1：8~1：10, loading flow velocity is 1BV/h, with 6BV water (elution speed 3BV/h), 4BV 30%
Ethanol (elution speed 2BV/h), the ethanol (elution speed 2BV/h) of 5BV 70% wash-out, collect 70% ethanol eluate, concentrate,
Dry, obtain sanchi leaf total saposins 71g, high performance liquid chromatography measures ginsenoside Rb3Content is 11.25%.
Embodiment 3, D101 macroreticular resin decoloration process optimizing research processes：
1st, the measure of static saturated adsorption capacity
Processed good D101 macroporous absorbent resin 10.0g are accurately weighed, is placed in 250ml conical flasks, accurately add three
Seven leaf upper prop liquid (ginsenoside Rb3Known to content) 200.0ml, standing adsorption 24h after fully shaking, filter, take subsequent filtrate
10ml, ginsenoside Rb is determined by content assaying method3Content, calculates D101 macroreticular resins at ambient temperature to ginsenoside
Rb3Saturated extent of adsorption.Adsorbance=[(concentration after concentration-absorption before absorption) * adsorption liquids volume]/resin quality, determines knot
Fruit is shown in Table 1.
2nd, static desorption experiment
10g D101 macroreticular resins after 24h Static Adsorptions, remove surface liquid, accurate to add 70% ethanol 100ml, fill
24h is stood after dividing shaking, saponin(e is fully desorbed, filtered, take subsequent filtrate 10ml, ginsenoside is determined by content assaying method
Rb3Content, calculates desorption efficiency.Desorption efficiency (%)=(solution solubility after solution solubility * desorptions after desorption)/[(the preceding concentration of absorption-
Concentration after absorption) * adsorption liquids volume] * 100%, measurement result is shown in Table 1.
The measure of the static saturated adsorption capacity of table 1 and desorption efficiency
In order to avoid causing the leakage loss of total saposins in production process, with 80% loading of resin adsorption amount, i.e., every gram
The ginsenoside Rb of D101 macroreticular resins3Applied sample amount must not exceed 11mg.
3rd, the selection of solvent is eluted
It is eluent to use ethanol-water system, 4 parts of the D101 macroreticular resins of sanchi leaf upper prop liquid saturation of learning from else's experience absorption, often
Part 50g, first with 4BV (column volume) water elution after, then respectively with 20%, 30%, 60%, 70%, 80% second of 4BV (column volume)
Alcohol is eluted, and collects eluent, and concentrate drying is prepared into suitable need testing solution, by ginsenoside Rb3Content assaying method is surveyed
Determine content, calculate the eluting rate of different concentration ethanol.With eluting solvent as abscissa, eluting rate is that ordinate draws parsing song
Line, is shown in Fig. 2.
Result shows, when concentration of alcohol be 30% and its it is following when, ginsenoside Rb3Eluting rate is very low, works as concentration of alcohol
When increasing to 70%, ginsenoside Rb3Eluting rate up to more than 90%, as concentration of alcohol is further added by, ginsenoside Rb3Eluting rate
Increases slowly, comprehensive production cost considers, therefore selection 30% and its following concentration ethanol are removal of impurities eluent, 70% ethanol is behaved
Ginseng saponin(e Rb3Target wash-out solution.
4th, confirmatory experiment
Sanchi leaf is taken, is divided into 3 parts, every part of 1kg, plus 15 times of 70% alcohol refluxs of amount are extracted 2 times, each 3h, extract solution mistake
Filter, merge, being concentrated into relative density 1.20 (60 DEG C), plus 5 times of amount water enter water-filling and sink, after standing 24h, filtering, filtrate is concentrated into
1.07~1.09 (60 DEG C), upper D101 macroreticular resins decolourize, blade diameter length ratio 1：8~1：10, loading flow velocity is 1BV/h, with 6BV water
The ethanol elution removal of impurities of (elution speed 3BV/h) and 4BV 25%, is finally eluted with 5BV70% ethanol (elution speed 2BV/h),
70% ethanol eluate is collected, is concentrated, dried, determine ginsenoside Rb in sanchi leaf total saposins3Content, the results are shown in Table 2.
23 batches of confirmatory experiment results of table
The result shows that sanchi leaf total saposins stable preparation process is feasible, quality controllable.
The comparing of embodiment 4, preparation method of the invention and existing method
Claims (10)
1. a kind of preparation method of sanchi leaf total saposins, it is characterised in that comprise the following steps：
1) solvent extraction will be used after sanchi leaf coarse crushing, pseudo-ginseng leaf extract will be obtained, the solvent be selected from water, 70% ethanol it is any one
Kind；
2) after gained pseudo-ginseng leaf extract inspissated juice relative density is 1.10~1.25 (60 DEG C), ethanol is added to make alcohol content extremely
50%~70% or add 3~7 times amount water enter water-filling sink, standing separation takes supernatant；
3) supernatant is decolourized by macroreticular resin, is first eluted with water and low-concentration ethanol, and 70% ethanol elution is used afterwards, is collected
Eluent, reclaims ethanol, and concentrate drying is obtained final product.
2. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that
Step 2) described in extract concentration be concentrated into relative density for 1.15~1.20 (60 DEG C)；
Step 2) described in ethanol final concentration of 55%~65%；
Step 2) described in water addition for 5~6 times amount.
3. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that
Step 3) described in macroreticular resin be D101 macroreticular resins；
Step 3) described in washing consumption be 3~6BV (column volume) consumption；
Step 3) described in low-concentration ethanol be 20%~30% ethanol；
Step 3) described in low-concentration ethanol consumption be 3~6BV (column volume) consumption；
Step 3) described in 70% ethanol consumption be 4~6BV consumptions.
4. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that comprise the following steps：
Take sanchi leaf 1kg, plus 10-20 times is measured 50-90% alcohol refluxs and extracted 1-3 time, each 2-4h, extract solution filtering, merging,
Concentration, plus 4-6 times measured water and enter water-filling and sink, and is stood, filtering, filtrate concentration, upper D101 macroreticular resins decolourize, with 6BV water and 4BV
25% ethanol elution removal of impurities, finally with the ethanol elutions of 5BV 70%, collects 70% ethanol eluate, and concentration is dried, and obtains three
Seven leaf total saposins.
5. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that comprise the following steps：
Sanchi leaf 1kg is taken, plus 10-20 times is measured water refluxing extraction 1-3 times, each 2-4h, extract solution merges concentration, plus ethanol makes to contain
Alcohol amount reaches 50-70%, stands, filtering, and filtrate concentration, upper D101 macroreticular resins decolourize, successively with 6BV water, the ethanol of 4BV 30%,
With the ethanol elutions of 5BV 70%, 70% ethanol eluate is collected, concentration is dried, and obtains sanchi leaf total saposins.
6. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that comprise the following steps：
Sanchi leaf 1kg is taken, plus 15 times of 70% alcohol refluxs of amount are extracted 2 times, each 3h, extract solution is filtered, merged, being concentrated into relatively
Density 1.20, plus 5 times of amount water enter water-filling and sink, and after standing 24h, filtering, filtrate is concentrated into 1.07~1.09, upper D101 macroreticular resins
Decolourize, blade diameter length ratio 1：8~1：10, with the ethanol elution removal of impurities of 6BV water and 4BV 25%, finally with the ethanol elutions of 5BV 70%,
70% ethanol eluate is collected, is concentrated, dried, obtain sanchi leaf total saposins.
7. sanchi leaf total saposins preparation method according to claim 1, it is characterised in that comprise the following steps：
Sanchi leaf 1kg is taken, plus 15 times are measured water refluxing extraction 2 times, each 3h, extract solution merging is concentrated into relative density 1.20, plus
Ethanol makes alcohol content up to 60%, and after standing 24h, filtering, filtrate is concentrated into 1.07~1.09, and upper D101 macroreticular resins decolourize, footpath
Height compares 1：8~1：10, loading flow velocity is 1BV/h, successively with 6BV water, the ethanol of 4BV 30%, the ethanol elutions of 5BV 70%, is collected
70% ethanol eluate, concentration is dried, and obtains sanchi leaf total saposins.
8. a kind of sanchi leaf total saposins, it is characterised in that obtained by one of claim 1~7 preparation method is made.
9. sanchi leaf total saposins described in claim 8 are preparing palpitaition, insomnia, chest caused by treating deficiency of heart-QI, the stagnation of the heart blood
Applied in pain, Chinese medicine preparation Qiyeshen' and tablet uncomfortable in chest.
10. the content assaying method of sanchi leaf total saposins, comprises the following steps：
Determined according to high performance liquid chromatography (four general rules 0512 of Chinese Pharmacopoeia version in 2015),
Chromatographic condition is tested with octadecylsilane chemically bonded silica as filler with system suitability；With acetonitrile as mobile phase A,
It is Mobile phase B with 0.2% phosphoric acid solution, the regulation according to the form below carries out gradient elution；Detection wavelength is 203nm, theoretical tray
Number presses ginsenoside Rb3Peak is calculated and should be not less than 6000,
The preparation of reference substance solution takes ginsenoside Rb3Appropriate reference substance, it is accurately weighed, plus ethanol is made every 1ml containing 0.5mg
Solution, obtains final product,
The preparation of need testing solution takes sanchi leaf total saposins 50mg, accurately weighed, puts in 10ml measuring bottles, is dissolved with ethanol and dilute
Release to scale, shake up, filter, take subsequent filtrate, obtain final product,
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, and obtains final product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108497302A (en) * | 2018-03-23 | 2018-09-07 | 广东日可威富硒食品有限公司 | A kind of selenium-enriched cordceps militaris noodles and preparation method thereof |
| CN109481483A (en) * | 2018-12-29 | 2019-03-19 | 云南金七制药有限公司 | Increase the method for saponin of Radix Notoginseng leaf Rb3 dissolution rate in sanchi leaf |
| CN109528671A (en) * | 2018-12-29 | 2019-03-29 | 云南金七制药有限公司 | Sanchi leaf drop pills of total saponin |
| CN114377048A (en) * | 2022-01-20 | 2022-04-22 | 云南金七制药有限公司 | Qiyeshenan dripping pill for treating insomnia and preparation method thereof |
| CN115792015A (en) * | 2022-12-06 | 2023-03-14 | 云南金七制药有限公司 | Quality detection method of Qiyeshenan dripping pills |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005341956A (en) * | 2004-06-07 | 2005-12-15 | Mitsuru Kudo | Method for producing refreshing drinking water by imparting natural deep sea water with functionality |
| CN103948659A (en) * | 2014-05-23 | 2014-07-30 | 云南维和药业股份有限公司 | Preparation method of notoginseng leaf total saponins |
-
2016
- 2016-12-22 CN CN201611196949.9A patent/CN106727806B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005341956A (en) * | 2004-06-07 | 2005-12-15 | Mitsuru Kudo | Method for producing refreshing drinking water by imparting natural deep sea water with functionality |
| CN103948659A (en) * | 2014-05-23 | 2014-07-30 | 云南维和药业股份有限公司 | Preparation method of notoginseng leaf total saponins |
Non-Patent Citations (4)
| Title |
|---|
| Y.HAN等: ""Microbial transformation of ginsenosides Rb1,Rb3,Rc by Fusarium sacchari"", 《JOURNAL OF APPLIED MICROBIOLOGY》 * |
| 吴少雄等: ""三七叶苷的提取分离与纯化"", 《食品与发酵工业》 * |
| 国家药典委员会: "《中华人民共和国药典：2015年版.一部》", 30 June 2015 * |
| 王兆华等: ""大孔树脂分离纯化三七叶总皂苷工艺的研究"", 《山东化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108497302A (en) * | 2018-03-23 | 2018-09-07 | 广东日可威富硒食品有限公司 | A kind of selenium-enriched cordceps militaris noodles and preparation method thereof |
| CN109481483A (en) * | 2018-12-29 | 2019-03-19 | 云南金七制药有限公司 | Increase the method for saponin of Radix Notoginseng leaf Rb3 dissolution rate in sanchi leaf |
| CN109528671A (en) * | 2018-12-29 | 2019-03-29 | 云南金七制药有限公司 | Sanchi leaf drop pills of total saponin |
| CN114377048A (en) * | 2022-01-20 | 2022-04-22 | 云南金七制药有限公司 | Qiyeshenan dripping pill for treating insomnia and preparation method thereof |
| CN114377048B (en) * | 2022-01-20 | 2022-10-21 | 云南金七制药有限公司 | Qiyeshenan dripping pill for treating insomnia and preparation method thereof |
| CN115792015A (en) * | 2022-12-06 | 2023-03-14 | 云南金七制药有限公司 | Quality detection method of Qiyeshenan dripping pills |
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