CN102058637A - Preparation method of patrimia scabiosaefolia extract - Google Patents
Preparation method of patrimia scabiosaefolia extract Download PDFInfo
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- CN102058637A CN102058637A CN201110024222.3A CN201110024222A CN102058637A CN 102058637 A CN102058637 A CN 102058637A CN 201110024222 A CN201110024222 A CN 201110024222A CN 102058637 A CN102058637 A CN 102058637A
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- patrinia scabiosaefolia
- coarse powder
- scabiosaefolia fisch
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- 238000002360 preparation method Methods 0.000 title abstract description 14
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- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000341 volatile oil Substances 0.000 claims abstract description 17
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- 238000005325 percolation Methods 0.000 claims abstract description 12
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- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 2
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- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method of a patrimia scabiosaefolia extract. The preparation method comprises the steps of: pulverizing cleaned patrimia scabiosaefolia raw materials into coarse powder; preparing a liquid mixture of water and volatile oil by adopting a stream distillation method; separating the liquid mixture to obtain patrimia scabiosaefolia volatile oil; drying the raw material coarse powder and immersing with an ethanol solution; adding an ethanol solution the weight of which is 15 times of the weight of the raw material coarse powder for percolation; collecting the percolate, decompressing and concentrating, and recovering ethanol; and adding the extracted volatile oil, and uniformly mixing to obtain the patrimia scabiosaefolia extract. The preparation method disclosed by the invention optimizes the percolation process, the yield of the obtained patrimia scabiosaefolia extract is increased greatly, and the content and the transfer rate of oleanolic acid are increased effectively and obviously. The patrimia scabiosaefolia extract has obvious effect on tranquilizing central nerves.
Description
Technical field
The present invention relates to nervus centralis medicine technical field, specifically, relate to a kind of preparation method that is used for nervus centralis abirritative preparation that from the Patrinia scabiosaefolia Fisch crude drug, extracts.
Background technology
In the time of social economy's fast development, people's living standard raising, social competition is also in continuous aggravation, severe employment situation and the operating pressure that continues to increase, be in for a long time in the ambient pressure of this anxiety, people are easy to enter " subhealth state " state, wherein the most significantly to surely belong to the insomnia be the neurasthenia or the mental sickness of cardinal symptom in performance, and according to statistics, population of China insomnia sickness rate is about 30%.
At present, the nervus centralis downern kind that is used for the treatment of insomnia is more, Western medicine mainly concentrates on Benzodiazepines diazepam, barbiturates such as quinalbarbitone and other class medicines such as zolpidem etc., and Chinese medicine mainly contains Rhizoma Acori Graminei and Baijiang Tablets, Qiyeshen an sheet, Helicid sheet or the like.Applicant initiative be that the Baijiang Tablets of major ingredient is included the earliest in " in one one of the Chinese pharmacopoeia of version in 1977 with the Patrinia scabiosaefolia Fisch, but be confined to condition at that time, this prescription is under the method for making item of Chinese Pharmacopoeia standard, only point out to adopt 60% ethanol to extract as the percolation of solvent, the dip time, percolation speed and the percolate that there is no in the clear and definite percolation process are collected process conditions such as dosage, thereby can not become standard production technology and instruct medicine production, all do not extract as the volatile oil of effective ingredient yet.In " standards of pharmacopoeia " of the Baijiang Tablets of producing simultaneously " discriminating " also have only three big class chromogenic reactions of plant component that specificity is not strong down, testing product that can not qualitative, quantitative makes the difficult quality guarantee of medicine.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, propose a kind of preparation method of producing feasible, process optimization and quality controllable Patrinia scabiosaefolia Fisch preparation.
Purpose of the present invention is achieved by following technical proposals.
* except as otherwise noted, used percent is percetage by weight among the present invention.
Patrinia scabiosaefolia Fisch preparation of the present invention is prepared from by Valerianaceae plant Patrinia scabiosaefolia Fisch Patrinia scabiosaefolia Fisch. rhizome and root.Herba Patriniae is a medicinal plants, its root and rhizome contain oleanolic acid, saponins, the main active constituents of medicine of volatilization wet goods, studies have shown that Patrinia scabiosaefolia Fisch has sedation, and think that wherein contained saponin is its effective ingredient, research simultaneously further proves that also the ethanol extract of Patrinia scabiosaefolia Fisch or volatile oil are oral, and mice is all had tangible sedation.
A kind of Patrinia scabiosaefolia Fisch extract making method, make by following step:
(1) pulverize: the Patrinia scabiosaefolia Fisch raw material after will making is only crossed 40 mesh sieves and is ground into coarse powder, and is standby;
(2) volatile oil extracts: adopt the vapor distillation method, obtain the liquid mixture of water and volatile oil, obtain Patrinia scabiosaefolia Fisch volatile oil after separating;
(3) moistening: will be through the Patrinia scabiosaefolia Fisch raw material coarse powder drying after the distillation, with concentration be 60% alcoholic solution as solvent, abundant moistening above-mentioned raw materials coarse powder left standstill 60 minutes;
(4) percolation: the raw material coarse powder after moistening is placed in the percolator, adds concentration and be 60%, gross weight is the alcoholic solution of 15 times of raw material coarse powder weight, flood after 24 hours, with 7ml/ minute flow velocity to its percolation and collection until finishing;
(5) the concentrated alcohol of receiving: will go up the percolate of collecting in the step and carry out concentrating under reduced pressure and reclaim ethanol, and promptly obtaining Patrinia scabiosaefolia Fisch extractum behind the volatile oil adding mixing that extracts in the step (2).Wherein, spissated temperature is less than 70 ℃, Steam Heating pressure≤0.2MPa, and the Patrinia scabiosaefolia Fisch extractum relative density that makes with this understanding is 1.10 ~ 1.20.
The practice of pharmacy of application of known adds different conventional adjuvants, can be prepared into various oral Pharmaceutical dosage forms, as tablet, granule, hard capsule, soft capsule, drop pill, concentrated pill, oral liquid and medicated wine.
With respect to prior art, the present invention has following beneficial effect:
1, the present invention adopts the vapor distillation method that raw material is extracted volatile oil, and it is joined that raw material coarse powder after the distillation continues with concentration is that 60% ethanol percolate extraction makes in the Patrinia scabiosaefolia Fisch extractum, and its active drug composition is fully used.
2, by the optimization to the percolation technical process, the Patrinia scabiosaefolia Fisch yield of extract that obtains improves greatly, and has increased the content of oleanolic acid effectively, and its rate of transform is significantly improved, and treatment nervus centralis sedation effect is remarkable.
3, differentiate the Herba Patriniae composition through the TLC method, with the content of HPLC method mensuration oleanolic acid, Patrinia scabiosaefolia Fisch extractum of the present invention all meets and has improved the quality control standard of Patrinia scabiosaefolia Fisch medicine.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment; but be to be understood that; embodiment only is an explanation of the invention; and limit the invention never in any form; various changes or modification that those skilled in the art do according to spirit of the present invention fall within protection scope of the present invention equally.
Embodiment 1
Take by weighing Patrinia scabiosaefolia Fisch raw material 1000g, it is standby that back 40 mesh sieves excessively of its clean system are ground into coarse powder; Adopt the vapor distillation method, the raw material coarse powder is put on the boiler sieve plate distilled, the mixture steam of generation imports the liquid mixture that obtains water and volatile oil in the condenser after the cooling along pot top gooseneck, obtains Patrinia scabiosaefolia Fisch volatile oil after separating; Will be through the Patrinia scabiosaefolia Fisch raw material coarse powder drying after the distillation (or after measuring moisture content be that 95% ethanol be adjusted to ethanol content be 60% with concentration), with concentration be 60% ethanol as solvent, abundant moistening above-mentioned raw materials coarse powder left standstill 60 minutes; Raw material coarse powder after moistening is placed in the percolator, adds concentration and be 60%, gross weight is the alcoholic solution of 15 times of raw material coarse powder weight, flood after 24 hours, with 7ml/ minute flow velocity to its percolation and collection until finishing; The percolate of collecting is carried out concentrating under reduced pressure and reclaims ethanol, obtain Patrinia scabiosaefolia Fisch extractum after adding Patrinia scabiosaefolia Fisch volatile oil mixing, wherein, 70 ℃ of thickening temperatures, Steam Heating pressure 0.2MPa, the Patrinia scabiosaefolia Fisch extractum relative density that makes with this understanding is 1.10 ~ 1.20.
Embodiment 2
Repeat embodiment 1, following difference is arranged: spissated temperature is 60 ℃, and Steam Heating pressure is 0.15MPa.
Embodiment 3
Repeat embodiment 1, following difference is arranged: spissated temperature is 50 ℃, and Steam Heating pressure is 0.1MPa.
Embodiment 4
Repeat embodiment 1, add concentration and be 90% alcoholic solution 10-50ml as dilution, starch 100-150g as disintegrating agent and 2-3g magnesium stearate as lubricant, make 1000 of Baijiang Tablets through granulation, drying, granulate, tabletting, coating sugar-coat or film-coat.
Embodiment 5
Repeat embodiment 1, add concentration and be 90% alcoholic solution 10-50ml as dilution, soluble starch 100-150g and Icing Sugar 300g through granulating, being packed as 500 bag Herba Patriniae granules after the drying.
Embodiment 6
Repeat embodiment 1, add concentration and be 90% alcoholic solution 10-50ml as dilution, soluble starch 100-150g as disintegrating agent and 2-3g magnesium stearate as lubricant, behind granulation, drying, granulate, filler capsule, make 1000 Herba Patriniae capsules.
Embodiment 7
Repeat embodiment 1, under 60 ℃ of conditions, dry, pulverize, it is joined mix homogeneously among the hot PEG4000 that melts, be incubated the degassing down in 80 ± 2 ℃ of temperature conditions; The degassing places this hybrid medicine in the drop pill machine after finishing, and regulates splashing into molding in the refrigerative simethicone, drips and makes the 0.1g/ grain, makes 3000 of Patrinai villosa dropping pills after removing the simethicone that shows.
Embodiment 8
Repeat embodiment 1, descended 100 mesh sieves to be ground into fine powder, add wetting agent water 10-50ml, binder starch 100-200g mix homogeneously is made soft material 60 ℃ of conditions, on roll the ball machine, be rolled into Herba Patriniae concentrated pill 2000 balls, dry.
Embodiment 9
Repeat embodiment 1, under 60 ℃ of conditions, be dried and crushed into micropowders, add the propylene glycol of 100-200g disperse medium PEG400 and 7%, adopt on the pressing, rotate rolling capsule machine automatically and make 1000 of Herba Patriniae soft capsules.
Embodiment 10
Repeat embodiment 1, add pure water and dissolve, leave standstill, filter, add correctives or sweeting agent mixing in filtrate, the water standardize solution is that 5000ml promptly gets the Herba Patriniae oral liquid.
Embodiment 11
Repeat embodiment 1, be 15% dissolve with ethanol, leave standstill, filter adding concentration, the ethanol standardize solution with 15% is that 5000ml promptly gets the Herba Patriniae medicated wine.
Test example 1Patrinia scabiosaefolia Fisch extractum of the present invention is to acute toxicity test in mice
The MID of the oral Patrinia scabiosaefolia Fisch extractum of mice is the 20g/kg body weight, is equivalent to 1000 times of clinical adult's consumption every day, does not see toxic reaction.
Test example 2The pharmacodynamics test of Patrinia scabiosaefolia Fisch extractum of the present invention
Animal experiment is discovered, Patrinia scabiosaefolia Fisch extractum among the embodiment 1 all has in various degree control to the autonomic activities of normal mouse and caffeine central excitation mice, the sleep rate of increase pentobarbital sodium hypnosis animal that can be in various degree, prolong dosage pentobarbital sodium mouse sleep time above threshold, prompting Patrinia scabiosaefolia Fisch extractum has tangible sedation.
Test example 3Patrinia scabiosaefolia Fisch extractum of the present invention is to the mice long term toxicity test
Rat be equivalent to clinical plan with 150 times of dosage, 100 times and 50 multiple doses under Patrinia scabiosaefolia Fisch extractum among the oral embodiment 1 observed for 12 weeks and reversibility observed for 2 weeks, the animal subject general state is good, respectively organize rat body weight during the administration and increase basically identical, routine blood test and blood biochemical detect and show that all said preparation all has no adverse effects to routine blood test, liver function, the renal function of animal subject, the main organs pathological examination there is no the pathological change relevant with drug toxicity, no Secondary cases toxic reaction changes after the drug withdrawal, points out this Patrinia scabiosaefolia Fisch extractum oral administration safety bigger.
Test example 4Patrinia scabiosaefolia Fisch extractum sheet of the present invention is used for clinical trial
Three hospital clinicals are tested 400 examples (test group 300 examples, matched group 100 examples), Patrinia scabiosaefolia Fisch group total effective rate 83.67%, and wherein clinical cure 3.67%, obvious effective rate 39.67%, effective percentage 40.33%; Neurasthenia's total effective rate 82% of matched group Helicid sheet, wherein clinical cure 5%, obvious effective rate 27%, effective percentage 50% has shown that Herba Patriniae extractum is insomnia for Cure for insomnia clinical efficacy is preferably arranged, and is outstanding to severe insomnia curative effect especially, and untoward reaction is slight, have no side effect, and can improve its concomitant symptom, other indivedual pathology can reach the degree of clinical cure.
Test example 5Patrinia scabiosaefolia Fisch extractum preparation technology effect of the present invention
The preparation process of Patrinia scabiosaefolia Fisch extractum of the present invention is made two levels, three factor orthogonal tests, the results are shown in Table 1.
Twice of each level test comprehensive scores and extreme difference are calculated, and result of calculation is listed in the table 2.
Table 2 is the surface as a result, the influence factor: quantity of solvent〉the infiltrating time table〉percolation speed.Experimental factor level result is as table 3.
Direct observation and from table 1 with reference to result calculated in the table 2, synopsis 3, A as can be known
2B
1C
2Be best conditions, illustrative experiment is for No. 3 an optimized process conditions, and higher yield of extract 16% is not only arranged, higher oleanolic acid content 0.4%, and the higher rate of transform 86.49% is arranged.
Test example 6The thin layer of Patrinia scabiosaefolia Fisch is analysed discriminating
Take by weighing Patrinia scabiosaefolia Fisch extractum 2g of the present invention, add alcoholic solution 20ml, cold, filtration that heating and refluxing extraction was put after 1 hour, with the filtrate evaporate to dryness, residue adds the 2ml alcoholic solution makes its dissolving, as need testing solution; Other gets Herba Patriniae medical material reference substance 1g, extracts as stated above and is prepared into reference substance solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same high-efficient silica gel G lamellae, mix the back as developing solvent with toluene-ethyl acetate-formic acid (15:2:0.5), launch, take out, dry, spray is 10% ethanol solution of sulfuric acid with concentration, it is clear to be heated to least bit colour developing at 105 ℃, places under the ultraviolet light (365nm) and inspects, in the test sample chromatograph, with the corresponding position of reference substance on, show the speckle of same color.
Conclusion: on 6 batches of test specimens and the corresponding position of reference substance Herba Patriniae medical material, showing the speckle of same color, serves as contrast when differentiating with the TLC method with the Patrinia scabiosaefolia Fisch medical material, and quantity of information is more, more problem can be described.
Test example 7The assay of oleanolic acid
Utilize according to high performance liquid chromatography and measure.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, and methanol-glacial acetic acid-triethylamine-water (87:0.03:0.015:13) is a mobile phase; The detection wavelength is 210nm, flow velocity 0.6ml/min, 30 ℃ of column temperatures.Theoretical cam curve is calculated by the oleanolic acid peak should be not less than 5000.
The preparation of reference substance solution: go the oleanolic acid reference substance an amount of, the accurate title, decide, and adds dissolve with methanol, makes every milliliter of solution that contains 0.14mg, in contrast the product test solution.
The preparation of need testing solution: the dried Patrinia scabiosaefolia Fisch extractum of the present invention of learning from else's experience is pulverized, the accurate title, decided 4.5g, puts in the band plug conical flask the accurate methanol 25ml that adds, claim to decide weight, supersound process 60 minutes is put coldly, supplies the weight of loss with methanol, shake up, leave standstill, get the supernatant filtering with microporous membrane, discard filtrate just, get subsequent filtrate as need testing solution.
Algoscopy: accurate respectively control sample solution and each 10 μ l of need testing solution of drawing, inject hplc determination promptly, the results are shown in table 4.
Show that from the measurement result of table 4 the present invention prepares that the optimization technology of Patrinia scabiosaefolia Fisch extractum is reliable, technical parameter is credible, and favorable reproducibility has reached the optimum state that Patrinia scabiosaefolia Fisch extracts.
Claims (3)
1. Patrinia scabiosaefolia Fisch extract making method, make by following step:
(1) pulverize: the Patrinia scabiosaefolia Fisch raw material after will making is only crossed 40 mesh sieves and is ground into coarse powder, and is standby;
(2) volatile oil extracts: adopt the vapor distillation method, the raw material coarse powder put on the boiler sieve plate distill, the mixture steam that produces imports the liquid mixture that obtains water and volatile oil in the condenser after the cooling along pot top gooseneck, obtains Patrinia scabiosaefolia Fisch volatile oil after separating;
(3) moistening: will be through the Patrinia scabiosaefolia Fisch raw material coarse powder drying after the distillation, with concentration be 60% alcoholic solution as solvent, abundant moistening above-mentioned raw materials coarse powder left standstill 60 minutes;
(4) percolation: the raw material coarse powder after moistening is placed in the percolator, adds concentration and be 60%, gross weight is the alcoholic solution of 15 times of raw material coarse powder weight, flood after 24 hours, with 7ml/ minute flow velocity to its percolation and collection until finishing;
(5) the concentrated alcohol of receiving: will go up the percolate of collecting in the step and carry out concentrating under reduced pressure and reclaim ethanol, and promptly obtaining Patrinia scabiosaefolia Fisch extractum behind the volatile oil adding mixing that extracts in the step (2).
2. the method for preparing Patrinia scabiosaefolia Fisch extractum according to claim 1 is characterized in that, in the described step (5) spissated temperature less than 70 ℃, Steam Heating pressure≤0.2MPa, the Patrinia scabiosaefolia Fisch extractum relative density that makes is 1.10 ~ 1.20.
3. the method for preparing Patrinia scabiosaefolia Fisch extractum according to claim 1, it is characterized in that, the practice of pharmacy of application of known adds different conventional adjuvants in described Patrinia scabiosaefolia Fisch extractum, be prepared into tablet, granule, hard capsule, soft capsule, drop pill, concentrated pill, oral liquid and medicated wine.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286056A (en) * | 2011-06-24 | 2011-12-21 | 苏州世林医药技术发展有限公司 | Oleanolic acid derivative and preparation method thereof |
| CN104523781A (en) * | 2015-01-10 | 2015-04-22 | 江西济民可信药业有限公司 | Preparation method for Baijiang cold pellets |
| CN106501440A (en) * | 2016-10-24 | 2017-03-15 | 中悦民安（北京）科技发展有限公司 | The discrimination method of field pennycress in Chinese medicine compound prescription |
| CN113057994A (en) * | 2021-04-09 | 2021-07-02 | 一力制药(南宁)有限公司 | Patrinia scabiosaefolia active component, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101342200A (en) * | 2008-06-14 | 2009-01-14 | 云南云河药业有限公司 | Patrinai villosa tablet and preparation method |
-
2011
- 2011-01-21 CN CN2011100242223A patent/CN102058637B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101342200A (en) * | 2008-06-14 | 2009-01-14 | 云南云河药业有限公司 | Patrinai villosa tablet and preparation method |
Non-Patent Citations (4)
| Title |
|---|
| 《中华人民共和国药典1999年版一部》 19951231 国家药典委员会 败酱片 522 1-3 * |
| 《中草药》 20101031 夏明文等 黄花败酱化学成分研究 1612-1615 1-3 第41卷, 第10期 * |
| 《北京中医杂志》 19820330 罗和春等 中药黄花败酱镇静安眠作用的临床观察与药理药化研究 30-33 1-3 , 第3期 * |
| 《河南大学学报》 20040228 田智勇等 黄花败酱和异叶败酱挥发油的研究 35-39 1-3 第23卷, 第1期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286056A (en) * | 2011-06-24 | 2011-12-21 | 苏州世林医药技术发展有限公司 | Oleanolic acid derivative and preparation method thereof |
| CN104523781A (en) * | 2015-01-10 | 2015-04-22 | 江西济民可信药业有限公司 | Preparation method for Baijiang cold pellets |
| CN104523781B (en) * | 2015-01-10 | 2018-01-12 | 江西济民可信药业有限公司 | A kind of white sauce cold granules preparation method |
| CN106501440A (en) * | 2016-10-24 | 2017-03-15 | 中悦民安（北京）科技发展有限公司 | The discrimination method of field pennycress in Chinese medicine compound prescription |
| CN113057994A (en) * | 2021-04-09 | 2021-07-02 | 一力制药(南宁)有限公司 | Patrinia scabiosaefolia active component, preparation method and application thereof |
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