CN103599178A - Preparation method of bacteriostatic herba elsholtziae oil - Google Patents
Preparation method of bacteriostatic herba elsholtziae oil Download PDFInfo
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- CN103599178A CN103599178A CN201310614194.XA CN201310614194A CN103599178A CN 103599178 A CN103599178 A CN 103599178A CN 201310614194 A CN201310614194 A CN 201310614194A CN 103599178 A CN103599178 A CN 103599178A
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Abstract
The invention relates to a preparation method for bacteriostatic herba elsholtziae oil. The preparation method comprises the following steps: (1) water vapour distillation: weighing 1 kilogram of herba elsholtziae, smashing, pouring into a distilling flash, adding water of which the weight is 10 times the weight of herba elsholtziae, installing a volatile oil extractor, carrying out steam distillation for 6 hours, pouring water-containing volatile oil into a separating from the volatile oil extractor, separating out a part of water-containing volatile oil, freezing at 10 DEG C below zero overnight in a refrigerator, removing ice to get the light yellow volatile oil, wherein the yield is 1.8%; and (2) weighing 1 kilogram of herba elsholtziae, smashing, putting the smashed herba elsholtziae in a 5L supercritical extraction kettle, starting the extraction kettle and a separating kettle heating device, starting a compression pump when a set temperature is reached, keeping cyclically extracting for 3h under the condition that the pressure in the extraction kettle is 20.0 MPa, the temperature in the extraction kettle is 50 DEG C, the flow velocity of CO2 in the extraction kettle is 40kg/h, the pressure and temperature of the separation kettle is 10.0 MPa and 30 DEG C respectively, thus obtaining a yellow oily substance which has special fragrance, wherein the extraction yield is 3%.
Description
Technical field
the invention belongs to medical technical field, be specifically related to the preparation method of antibacterial Herba Moslae oil.
Background technology
because causing the continuous rising of drug resistance, abuse of antibiotics become one of common difficult problem of paying close attention in the whole world at present.Especially the resistant rate of staphylococcus aureus has reached 90%, and the enteric flora disturbance that antibiotics causes simultaneously, also increases the weight of primary infection, finds anti-infectives from natural product, has realistic meaning.Herba Moslae Elsholtzia densa Benth. is Labiatae Elsholtzia species, is distributed in the provinces and regions such as Yunnan Province of China, Hebei, Shanxi, Shaanxi, Gansu, Qinghai, Sichuan, Tibet, Xinjiang.In Tibet, for Herba Moslae use, holding concurrently can be outward for dermatosis.
at present the composition of the volatile oil of Herba Moslae is had been reported, such as use extraction by steam distillation Herba Moslae volatile oils such as Zhang Ji and by gas chromatography/mass spectrometry technology, it is analyzed, identify and confirmed 84 kinds of compounds wherein, the 88.34%. main chemical compositions that its content accounts for full oil is germacrene (18.83%), D-limonene (11.17%), 2, 5, 5-tri-or four base-1, 3, 6-heptantriene (6.30%), 6-methylene-dicyclo [3, 1, 0], hexane (5.90%), caryophyllene oxide (3.94%), caryophyllene (3.36%), 4-carbon-3, 5-dimethyl hexamethylene-1-alkene (2.88%), α-3-cyclohexene-1-alcohol (2.06%).Pharmacological research to Herba Moslae volatile oil has no report.
the present invention relates to have the Herba Moslae volatile oil of antibacterial, antiviral and choline esterase inhibition and there is the application in antibacterial, antiviral and treatment alzheimer disease product in preparation, filled up the blank of Herba Moslae in this field application.
Summary of the invention
for the problems referred to above, the present invention aims to provide a kind of preparation method of antibacterial Herba Moslae oil.
a kind of preparation method of antibacterial Herba Moslae oil, comprise the following steps: (1) steam distillation: take Herba Moslae medical material 1kg, pulverize, join in alembic, add 10 times of amounts of water, volatile oil extractor is installed, vapor distillation 6 hours, from volatile oil extractor is heavy by moisture volatile oil separatory funnel, separate and reply a part, put into-10 ℃ of refrigerator and cooled and freeze and spend the night, water intaking deicing obtains light yellow volatile oil, yield 1.8%.
(2) take Herba Moslae 1kg, pulverize, be placed in 5L supercritical extraction reactor, open extraction kettle and separating still heating apparatus, after reaching design temperature, open compressor pump, make extraction kettle pressure remain 20.0MPa, temperature is 50 ℃, with the C02 flow velocity cycling extraction of 40kg/h.Separating still pressure and temperature is respectively 10.0MPa and 30 ℃, and cycling extraction 3 hours, obtains yellow oil, has peat-reek, is antibacterial Herba Moslae oil, and extraction ratio is 3%.
2. Herba Moslae volatile oil chemical composition of the present invention
gained Herba Moslae volatile oil is analyzed through GC-MS, and gas chromatography-mass spectrography technology gained mass spectrum as calculated machine mass spectrometric data library searching has been determined some chemical properties in Herba Moslae volatile oil.GC conditions: quartz capillary column VarianVF-5MS CP8944,30m * 0.25mm, thickness 0.25 μ m.Heating schedule: since 60 ℃, be raised to 250 ℃ with 5 ℃/min, then be raised to 280 ℃ with 15 ℃/min, carrier gas is He, post flow 1.0mL/min, 270 ℃ of injector temperatures.Mass spectrum condition: EI power supply; Ionization voltage 70eV; 230 ℃ of ion source temperatures; Sweep limits 30～550aum; Sample size 1 μ l, split ratio: 22: 1.Analysis and Identification structure shows, Herba Moslae volatile oil main chemical compositions is patchouli alcohol (13.82%), 2, 4-diethyl acrylic-1-methyl isophthalic acid-vinyl cyclohexane (9.04%), decahydro-4a-methyl isophthalic acid-methylene-7-(1-the first and second bases)-naphthalene alkene (8.97%), 1, 2, 3, 3a, 4, 5, 6, 7-octahydro-1, 4-dimethyl-7-(1-the first and second bases)-azulene (6.37%), 1, 2, 3, 4, 5, 6, 7, 8-octahydro 1, 4-dimethyl-7 (1-the first and second bases)-azulene (5.92%), 5-epoxy isopropyl allyl acetic acid (5.21%), Patchoulene (3.96%), ylangene (3.90%), 1, 2, 3, 3a, 4, 5, 6, 7-octahydro-. α, α, 3, 8-tetramethyl-5-azulene methanol (3.27%), caryophyllene (2.15%), 2, 6, 6-trimethyl-1-epoxy hexene-1-acetaldehyde (2.12%), 1, 2, 3, 5, 6, 7, 8, 8a-octahydro-1, 8a-dimethyl-7-(1-the first and second bases)-naphthalene alkene (2.02%) etc., total content accounts for 84.59% of full oil.
the experiment proved that, Xinjiang Herba Moslae volatile oil, has broad-spectrum antibacterial, antivirus action, and Herba Moslae volatile oil is to antibacterials such as staphylococcus, escherichia coli genus, Rhodopseudomonass; Candida all has certain inhibition growth.Especially common bacteria pathogen staphylococcus aureus is there is the effect of very strong inhibition growth, Candida albicans is there is to the effect of stronger inhibition growth.Therefore, Xinjiang Herba Moslae volatile oil can be applicable to the industries such as food, medicine, health product, cosmetics, prepares the various forms of products with bacteriostasis.
The specific embodiment
below in conjunction with specific embodiment, the present invention is described in further details.
the preparation method of a kind of Herba Moslae: (1) steam distillation: take Herba Moslae medical material 1kg, pulverize, join in alembic, add 10 times of amounts of water, volatile oil extractor is installed, vapor distillation 6 hours, from volatile oil extractor is heavy, by moisture volatile oil separatory funnel, separates and reply a part, put into-10 ℃ of refrigerator and cooled and freeze and spend the night, water intaking deicing obtains light yellow volatile oil, yield 1.8%.
(2) take Herba Moslae 1kg, pulverize, be placed in 5L supercritical extraction reactor, open extraction kettle and separating still heating apparatus, after reaching design temperature, open compressor pump, make extraction kettle pressure remain 20.0MPa, temperature is 50 ℃, with the C02 flow velocity cycling extraction of 40kg/h.Separating still pressure and temperature is respectively 10.0MPa and 30 ℃, and cycling extraction 3 hours, obtains yellow oil, has peat-reek, and extraction ratio is 3%.
method of testing: mdck cell is inoculated 96 well culture plates, puts 5%CO2,37C cultivates 24 hours.Mdck cell adds respectively influenza A type virus (15/90) 10-5, influenza B virus (13/97) 1/210-2, and 37 ℃ of absorption hypsokinesis in 2 hours venom of preventing or cure a disease, adds respectively different dilution factor medicines.If virus control and cell contrast, 37C cultivates 40 hours, and observed result, records CPE, calculates each sample resisiting influenza virus half-inhibition concentration (IC50).
the above; it is only preferred embodiment of the present invention; not in order to limit the present invention, any trickle modification that every foundation technical spirit of the present invention is done above embodiment, be equal to and replace and improve, within all should being included in the protection domain of technical solution of the present invention.
Claims (1)
1. the preparation method of an antibacterial Herba Moslae oil: it is characterized in that, comprise the following steps: (1) steam distillation: take Herba Moslae medical material 1kg, pulverize, join in alembic, add 10 times of amounts of water, volatile oil extractor is installed, vapor distillation 6 hours, from volatile oil extractor is heavy by moisture volatile oil separatory funnel, separate and reply a part, put into-10 ℃ of refrigerator and cooled and freeze and spend the night, water intaking deicing obtains light yellow volatile oil, yield 1.8%; (2) take Herba Moslae 1kg, pulverize, be placed in 5L supercritical extraction reactor, open extraction kettle and separating still heating apparatus, after reaching design temperature, open compressor pump, make extraction kettle pressure remain 20.0MPa, temperature is 50 ℃, with the C02 flow velocity cycling extraction of 40kg/h, separating still pressure and temperature is respectively 10.0MPa and 30 ℃, cycling extraction 3 hours, obtain yellow oil, have peat-reek, be antibacterial Herba Moslae oil, extraction ratio is 3%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105685129A (en) * | 2016-02-01 | 2016-06-22 | 孙爱华 | Medical disinfection liquid and preparation method thereof |
| CN108567814A (en) * | 2018-04-27 | 2018-09-25 | 江西中医药大学 | A kind of Herba Moslae volatile oil is for sterilizing and/or antibacterial, antimicrobial agent application and preparation method thereof |
| CN113173928A (en) * | 2021-04-25 | 2021-07-27 | 武汉国粹医药科技有限公司 | Terpenoid, preparation method and application thereof, and antibacterial agent |
| CN113416609A (en) * | 2021-07-22 | 2021-09-21 | 宿州学院 | High-quality elsholtzia plant volatile oil and efficient preparation method thereof |
| CN114306501A (en) * | 2020-09-28 | 2022-04-12 | 石家庄以岭药业股份有限公司 | Antibacterial and antiviral traditional Chinese medicine composition containing fritillaria and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451228A (en) * | 2010-10-26 | 2012-05-16 | 中国医学科学院药用植物研究所 | Preparation method and application of antibacterial and antiviral elsholtzia densa benth volatile oil |
-
2013
- 2013-11-27 CN CN201310614194.XA patent/CN103599178A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451228A (en) * | 2010-10-26 | 2012-05-16 | 中国医学科学院药用植物研究所 | Preparation method and application of antibacterial and antiviral elsholtzia densa benth volatile oil |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105685129A (en) * | 2016-02-01 | 2016-06-22 | 孙爱华 | Medical disinfection liquid and preparation method thereof |
| CN108567814A (en) * | 2018-04-27 | 2018-09-25 | 江西中医药大学 | A kind of Herba Moslae volatile oil is for sterilizing and/or antibacterial, antimicrobial agent application and preparation method thereof |
| CN114306501A (en) * | 2020-09-28 | 2022-04-12 | 石家庄以岭药业股份有限公司 | Antibacterial and antiviral traditional Chinese medicine composition containing fritillaria and preparation method and application thereof |
| CN113173928A (en) * | 2021-04-25 | 2021-07-27 | 武汉国粹医药科技有限公司 | Terpenoid, preparation method and application thereof, and antibacterial agent |
| CN113173928B (en) * | 2021-04-25 | 2022-05-27 | 武汉国粹医药科技有限公司 | Terpenoid, preparation method and application thereof and antibacterial agent |
| CN113416609A (en) * | 2021-07-22 | 2021-09-21 | 宿州学院 | High-quality elsholtzia plant volatile oil and efficient preparation method thereof |
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Application publication date: 20140226 |