CN105395618A - Method for extracting essential oil of Hui nationality drug prescription for treating stroke - Google Patents

Method for extracting essential oil of Hui nationality drug prescription for treating stroke Download PDF

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Publication number
CN105395618A
CN105395618A CN201610010472.4A CN201610010472A CN105395618A CN 105395618 A CN105395618 A CN 105395618A CN 201610010472 A CN201610010472 A CN 201610010472A CN 105395618 A CN105395618 A CN 105395618A
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extraction
volatile oil
medicinal powder
temperature
returns
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张立明
张万年
张霞
付雪艳
管恩爽
李姣宁
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Ningxia Medical University
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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)
    • A61K36/67—Piperaceae (Pepper family), e.g. Jamaican pepper or kava
    • 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)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/286—Carthamus (distaff thistle)
    • 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)
    • A61K36/32—Burseraceae (Frankincense family)
    • A61K36/328—Commiphora, e.g. mecca myrrh or balm of Gilead
    • 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)
    • A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a method for extracting essential oil of a Hui nationality drug prescription for treating stroke. The Hui nationality drug prescription is formed by pepper, piper longum, myrrh, cinnamon and safflower carthamus; the method comprises the following steps: pulverizing medicinal materials in the Hui nationality drug prescription into preset mesh numbers by using a pulverizer, so as to obtain medicinal material powder, and sealing the medicinal material powder; putting the medicinal material powder into a charging barrel, putting into an extraction kettle, and performing extraction on the medicinal material powder by adopting a supercritical CO2 extraction method, so as to obtain the corresponding essential oil, wherein extraction pressure is 20mpa to 30mpa, an extraction temperature is 40 DEG C to 55 DEG C, and extraction time is 20min to 120min.

Description

Treatment apoplexy returns the extracting method of prescription agent volatile oil
Technical field
The present invention relates to Chinese medicine ingredients abstraction technique field, particularly a kind ofly treat the extracting method that apoplexy returns prescription agent volatile oil.
Background technology
Apoplexy is apoplexy again, is the general designation of Chinese medicine to acute cerebrovascular disease, and be one of common cardiovascular and cerebrovascular disease, apoplexy is divided into ischemia and hemorrhage two kinds, and wherein cerebral infarction incidence rate accounts for 60% ~ 80%.Because Cerebral Haemorrhage Invasion Rate is high, mortality rate is high, disability rate is high, relapse rate is high and complication is many, so medical circle is listed as one of three large diseases threatening human health its same coronary heart disease, cancer.
Hui ethnic group's medical science is the national rich cultural heritages of the Huis, wherein incense drug is back the characteristic of medicine, incense drug is rich in volatile oil, usually giving out a sweet perfume property abnormal smells from the patient, there is effect of causing resuscitation with aromatic drugs, evident in efficacy to cerebral ischemia, main play its priming up, enter effect in brain fast, reach effect of causing resuscitation with aromatic drugs, blood circulation promoting and blood stasis dispelling.Such as, by on the basis of attached Hui Yi hospital of Ningxia Medical University based on Huihui Formularieses such as side, Radix Aucklandiae oil sides in the treatment Zha Linu think of side of apoplexy, Ha Heili, and through Empirical formula that clinical application for many years filters out: this Empirical formula is made up of Fructus Piperis, Piper longum, Myrrha, Cortex Cinnamomi, Flos Carthami, this Empirical formula main pharmacodynamics composition all has the pharmacological actions such as blood circulation promoting and blood stasis dispelling, anti-atherogenic be hard, and it is evident in efficacy.
The prior art also not extraction process of volatile oil in this apoplexy Huihui Formularies, can not realize its maximized medical value, this limits it to a certain extent and applies.Because the party is Chinese medicine compound, in order to maximum extracts effective ingredient, grinding medicinal materials is mixed extraction after powder, uses vapor extraction volatile oil before, but backflow causes the minimizing of effective ingredient for a long time, greatly reduces the drug effect of this Empirical formula.
Summary of the invention
In view of this, be necessary to provide a kind of can efficiently and the treatment apoplexy comprehensively extracting the volatile oil of above-mentioned Empirical formula Chinese medicine returns the extracting method of prescription agent volatile oil.
Treat the extracting method that apoplexy returns prescription agent volatile oil, this time prescription agent is made up of Fructus Piperis, Piper longum, Myrrha, Cortex Cinnamomi, Flos Carthami, and the method comprises the following steps:
Utilize pulverizer to be predetermined order number by the pulverizing medicinal materials of returning in prescription agent, to obtain medicinal powder, sealed by medicinal powder, ambient temperature when wherein pulverizing is 25 DEG C, and the power of pulverizer is 1200W.
Medicinal powder is loaded barrel, puts into extraction kettle, adopt supercritical CO 2extraction mode extracts medicinal powder, and to obtain corresponding volatile oil, wherein extracting pressure is 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, extraction time 20min ~ 120min.
Preferably, predetermined order number is 40 orders.
Preferably, extracting pressure is 25mpa.
Preferably, extraction temperature is 50 DEG C.
Preferably, extraction time is 100min.
Preferably, " medicinal powder is loaded barrel, puts into extraction kettle, adopt supercritical CO 2extraction mode extracts medicinal powder, to obtain corresponding volatile oil, wherein extracting pressure is 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, extraction time 20min ~ 120min " step be specially: by the medicinal powder of scheduled volume load barrel; put into extraction kettle, open SAPMAC method refrigeration air valve, arrange extraction kettle be separated I, be separated II temperature; When refrigeration plant is down to 4 DEG C, open high-pressure pump, and open respective valves maintenance channel status, regulate CO by effusion meter 2flow; Keep constant temperature and pressure circulate and maintain the scheduled time, extract complete, open separating still blow-off valve, collect extract.
Above-mentioned treatment apoplexy returns in the extracting method of prescription agent volatile oil, consider back that a few taste medicines in prescription agent all belong to hot dry drug in time medicine four property, and its volatile oil component is complicated, by keep ambient temperature when pulverizing the power of 25 DEG C and pulverizer be 1200W prevent oil components from volatilizing and powder adhesion paste the chamber wall of pulverizer situation occur, and adopt sealing means to preserve the medicinal powder pulverized, be extracting pressure by condition be again 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, the supercritical CO of extraction time 20min ~ 120min 2extraction mode extracts medicinal powder, to obtain corresponding volatile oil, adopt GC-MS to analyze, obtain 40 kinds of compositions altogether, identify 21 kinds of compositions, account for 44% of total composition, the trans-cinnamic aldehyde (9.14%) that mass fraction is higher, β-caryophyllene (3.21%), α-bisabolol (3.11%), β-heerabolene (2.56%), visible above-mentioned treatment apoplexy returns the extracting method of prescription agent volatile oil can efficiently and comprehensively extract the volatile oil of above-mentioned Empirical formula Chinese medicine.
Accompanying drawing explanation
Fig. 1 cinnamic aldehyde standard curve.
Fig. 2 is that grinding particle size affects result figure to apoplexy side's volatile oil extraction yield.
Fig. 3 is that extracting pressure affects result figure to apoplexy side's volatile oil extraction yield.
Fig. 4 is that extraction temperature affects result figure to apoplexy side's volatile oil extraction yield.
Fig. 5 is that extraction time affects result figure to apoplexy side's volatile oil extraction yield.
Fig. 6 is the total ion figure of volatile oil.
Fig. 7 is apoplexy side's volatile oil component and relative amount.
Detailed description of the invention
Treatment apoplexy provided by the invention returns the extracting method of prescription agent volatile oil, and this time prescription agent is made up of Fructus Piperis, Piper longum, Myrrha, Cortex Cinnamomi, Flos Carthami, and the method comprises the following steps:
Step S101, utilize pulverizer to be predetermined order number by the pulverizing medicinal materials of returning in prescription agent, to obtain medicinal powder, sealed by medicinal powder, ambient temperature during pulverizing is at 25 DEG C, and the power of pulverizer is 1200W.
Step S102, loads barrel by medicinal powder, puts into extraction kettle, adopts supercritical CO 2extraction mode extracts medicinal powder, and to obtain corresponding volatile oil, wherein extracting pressure is 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, extraction time 20min ~ 120min.This step is specially: the medicinal powder of scheduled volume is loaded barrel, puts into extraction kettle, opens SAPMAC method refrigeration air valve, arranges extraction kettle and is separated I, is separated the temperature of II; When refrigeration plant is down to 4 DEG C, open high-pressure pump, and open respective valves maintenance channel status, regulate CO by effusion meter 2flow; Keep constant temperature and pressure circulate and maintain the scheduled time, extract complete, open separating still blow-off valve, collect extract.
Above-mentioned treatment apoplexy returns in the extracting method of prescription agent volatile oil, consider back that a few taste medicines in prescription agent all belong to hot dry drug in time medicine four property, and its volatile oil component is complicated, by keep ambient temperature when pulverizing the power of 25 DEG C and pulverizer be 1200W prevent oil components from volatilizing and powder adhesion paste the chamber wall of pulverizer situation occur, and adopt sealing means to preserve the medicinal powder pulverized, be extracting pressure by condition be again 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, the supercritical CO of extraction time 20min ~ 120min 2extraction mode extracts medicinal powder, to obtain corresponding volatile oil, adopt GC-MS to analyze, obtain 40 kinds of compositions altogether, identify 21 kinds of compositions, account for 44% of total composition, the trans-cinnamic aldehyde (9.14%) that mass fraction is higher, β-caryophyllene (3.21%), α-bisabolol (3.11%), β-heerabolene (2.56%), visible above-mentioned treatment apoplexy returns the extracting method of prescription agent volatile oil can efficiently and comprehensively extract the volatile oil of above-mentioned Empirical formula Chinese medicine.
Illustrate that above-mentioned treatment apoplexy returns the extracting method technique effect of prescription agent volatile oil due to prior art, referring to Fig. 1 to Fig. 7 below by way of experimental analysis:
1 material and instrument
Material: the medical material returning prescription agent for the treatment of apoplexy: Fructus Piperis, Fructus Piperis Longi, Myrrha, Cortex Cinnamomi, Flos Carthami; CO 2(>=99%), methanol, analytical pure.
Instrument: supercritical CO 2extraction equipment (application separation company of the U.S.), Agilent6890N gas chromatograph (Agilent company of the U.S.), electronic analytical balance (prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit Instrument Ltd.), Shimadzu makings analytical chromatograph (Shimadzu QP2010Plus, 30*0.25mm, 0.25um), Constant Temp. Oven (the permanent tech equipment company limited in Shanghai one), abbe's refractometer (upper Nereid's tech device company limited)
2. method
The extraction of 2.1 volatile oil accurately takes the medical material after pulverizing in prescription ratio and loads barrel; put into extraction kettle; open SAPMAC method refrigeration air valve; arrange extraction kettle to be separated I, to be separated the temperature of II; when refrigeration plant is down to 4 DEG C; open high-pressure pump, and open respective valves maintenance channel status, regulated the flow of CO2 by effusion meter; Keep constant temperature and pressure circulate and maintain appropriate time, extract complete, open separating still blow-off valve, collect extract.Gas chromatography determination cinnamic aldehyde content.
2.2GC chromatographic condition U.S. Agilent 6890N gas chromatograph, HP-5MS type quartz capillary column (30.0m × 320 μm × 0.25 μm), carrier gas is high pure nitrogen, post flow 1.2ml/min, heating schedule: column temperature 50 DEG C keeps one minute, 150 DEG C are raised to 8 DEG C of speed per minute, keeping 3 minutes, being raised to 210 DEG C with 3 DEG C of speed per minute, keeping 5 minutes, being raised to 240 DEG C with 5 DEG C of speed per minute, keep 15 minutes.Injector temperature 250 DEG C, detector temperature 280 DEG C.Sample size 0.2 μ L.Split ratio: 20:1.
2.3GC/MS condition GC conditions: Agilent6890N gas chromatograph, Rxi-5silMS capillary chromatographic column (30m*0.25,0.25um); Injector temperature 250 DEG C, heating schedule: initial 50 DEG C, keeps 1min, rises to 120 DEG C with 10 DEG C/min, keeps 3min, rises to 200 DEG C with 3 DEG C/min, keeps 3min, rises to 290 DEG C with 5 DEG C/min, keeps 10min.Carrier gas is 99.999% helium, volume flow 1.0ml/min, sample size 1ul, split ratio 25:1.
Mass Spectrometry Conditions: EI ionization source, ion source temperature 230 DEG C, interface temperature 320 DEG C, quality of scanning scope m/z33-500.
The drafting precision absorption cinnamic aldehyde reference substance of 2.4 cinnamic aldehyde standard curves is appropriate, the reference substance of 2.98mg/ml is made with methanol, above-mentioned reference substance is diluted respectively 5 times, 10 times, 20 times, 30 times, 40 times, make series of standards product solution, enter chromatographic, draw the standard curve of cinnamic aldehyde content: y=233.76x-4.1337, R2=0.9999.Cinnamic aldehyde is good linear relationship between 0.0745mg-2.98mg.
2.5 experiment of single factor preliminary experiments in early stage find, volatile oil yield selects grinding particle size, extracting pressure, extraction temperature, extraction time to have relation with it, therefore first investigate by experiment of single factor the process conditions extracting volatile oil.
2.5.1 grinding particle size is on the impact of volatile oil extraction yield by " 2.1 " method, if pulverizing medicinal materials granularity is 20 orders, 40 orders, 60 orders, extraction temperature 45 degree, extracting pressure 25mpa, extraction time 100min, weigh and calculate extraction yield.
2.5.2 extracting pressure is on the impact of volatile oil extraction yield by " 2.1 " method, and fixing grinding particle size, if extracting pressure is 20mpa, 25mpa, 30mpa, 35mpa, extraction temperature 45 degree, extraction time is 100min, weighs and calculates extraction ratio.
2.5.3 extraction temperature on the impact of volatile oil extraction yield by " 2.1 " method, fixing grinding particle size, extracting pressure, if extraction temperature be temperature 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, extraction time is 100min, weighs and calculates extraction ratio.
2.5.4 extraction time is on the impact of volatile oil extraction yield by " 2.1 " method, and fixing grinding particle size, extracting pressure, extraction temperature, extraction time are that 20min, 40min, 60min, 80min, 100min, 120min weigh and calculate extraction ratio.
2.6 orthogonal experiments are according to experiment of single factor results, and with volatile oil yield and cinnamic aldehyde content for index, choose extracting pressure (A), extraction temperature (B), extraction time (C) investigate, each factor gets 3 horizontal experimental programs.
Table 1 quadrature factor water-glass
By table 1 factor level, use L 9(3 4) orthogonal experiment arrangement, investigate with volatile oil yield and cinnamic aldehyde content aggregative indicator, each experiment is number parallel does 3 experiments, the results are shown in Table 2.Result is carried out variance analysis, the results are shown in Table 3.
The supercritical extraction orthogonal test of table 2 volatile oil
Table 3 analysis of variance table
Note * F 0.05(2,2)=19; * F 0.01(2,2)=99
Intuitive analysis is known, and the impact order of each factor on extraction process is B > A > C, i.e. secondly pressure having the greatest impact to effect of extracting be temperature.Variance analysis shows, the impact of factor B on volatile oil yield has statistical significance, extraction temperature and time then there was no significant difference.In conjunction with single factor test, determine that optimum condition is A 2b 3c 2, i.e. extracting pressure 30mpa, temperature 50 C, time 100min.
2.7 confirmatory experiments take medicinal powder, and carry out 3 confirmatory experiments by optimum extraction process, result volatile oil yield is high, cinnamic aldehyde content is 2.01mg/g, 2.04mg/ml, 1.96mg/ml, RSD=1.81, than orthogonal any one group high, illustrates that the SFE-CO2 technologic study optimized is reliable and stable.
2.8GC-MS analyzes totally 40 kinds of compositions, identifies 21 kinds of compositions, accounts for 44% of total composition, the trans-cinnamic aldehyde (9.14%) that mass fraction is higher, β-caryophyllene (3.21%), α-bisabolol (3.11%), β-heerabolene (2.56%) etc.What discovery volatile oil content was the highest is cinnamic aldehyde and a non-principal component, and research thinks that cinnamic aldehyde has the effect of blood vessel dilating and blood pressure lowering.So choose cinnamic aldehyde to be that to carry out process optimization be rational to index composition.The important reference that the research that GC-MS result is seminar's later stage effective ingredient and pharmacological action thereof provides.

Claims (6)

1. treat the extracting method that apoplexy returns prescription agent volatile oil, this time prescription agent is made up of Fructus Piperis, Piper longum, Myrrha, Cortex Cinnamomi, Flos Carthami, and the method comprises the following steps:
Utilize pulverizer to be predetermined order number by the pulverizing medicinal materials of returning in prescription agent, to obtain medicinal powder, sealed by medicinal powder, ambient temperature when wherein pulverizing is 25 DEG C, and the power of pulverizer is 1200W.
Medicinal powder is loaded barrel, puts into extraction kettle, adopt supercritical CO 2extraction mode extracts medicinal powder, and to obtain corresponding volatile oil, wherein extracting pressure is 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, extraction time 20min ~ 120min.
2. treatment apoplexy as claimed in claim 1 returns the extracting method of prescription agent volatile oil, it is characterized in that: predetermined order number is 40 orders.
3. treatment apoplexy as claimed in claim 1 returns the extracting method of prescription agent volatile oil, it is characterized in that: extracting pressure is 25mpa.
4. treatment apoplexy as claimed in claim 1 returns the extracting method of prescription agent volatile oil, it is characterized in that: extraction temperature is 50 DEG C.
5. treatment apoplexy as claimed in claim 1 returns the extracting method of prescription agent volatile oil, it is characterized in that: extraction time is 100min.
6. treatment apoplexy as claimed in claim 1 returns the extracting method of prescription agent volatile oil, it is characterized in that: " medicinal powder is loaded barrel, puts into extraction kettle, adopt supercritical CO 2extraction mode extracts medicinal powder, to obtain corresponding volatile oil, wherein extracting pressure is 20mpa ~ 35mpa, extraction temperature 40 DEG C ~ 55 DEG C, extraction time 20min ~ 120min " step be specially: by the medicinal powder of scheduled volume load barrel; put into extraction kettle, open SAPMAC method refrigeration air valve, arrange extraction kettle be separated I, be separated II temperature; When refrigeration plant is down to 4 DEG C, open high-pressure pump, and open respective valves maintenance channel status, regulate CO by effusion meter 2flow; Keep constant temperature and pressure circulate and maintain the scheduled time, extract complete, open separating still blow-off valve, collect extract.
CN201610010472.4A 2016-01-08 2016-01-08 Method for extracting essential oil of Hui nationality drug prescription for treating stroke Pending CN105395618A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107446701A (en) * 2017-07-31 2017-12-08 青海民族大学 A kind of method of the Chinese medicine composition volatile oil and preparation method thereof with preparing Chinese medicine composition
CN109456830A (en) * 2018-11-27 2019-03-12 河南羚锐制药股份有限公司 The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107446701A (en) * 2017-07-31 2017-12-08 青海民族大学 A kind of method of the Chinese medicine composition volatile oil and preparation method thereof with preparing Chinese medicine composition
CN109456830A (en) * 2018-11-27 2019-03-12 河南羚锐制药股份有限公司 The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material

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Application publication date: 20160316

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