CN101933976A - Method for preparing nanoemulsion from high-efficient active sites of fructus forsythiae essential oil - Google Patents
Method for preparing nanoemulsion from high-efficient active sites of fructus forsythiae essential oil Download PDFInfo
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- CN101933976A CN101933976A CN 201010275253 CN201010275253A CN101933976A CN 101933976 A CN101933976 A CN 101933976A CN 201010275253 CN201010275253 CN 201010275253 CN 201010275253 A CN201010275253 A CN 201010275253A CN 101933976 A CN101933976 A CN 101933976A
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Abstract
The invention relates to a method for separating high-efficient anti-pathogenic microorganism active sites from fructus forsythiae essential oil and preparing the high-efficient active sites into nanoemulsion. The method relates to the separation of high-efficient active sites of fructus forsythiae essential oil and the preparation of nanoemulsion, and concretely comprises the following steps: separating through a functional graphene oxide or a low-pressure decompression fractionation method to obtain different active sites of fructus forsythiae essential oil; screening the active sites through antibiotic or anti-virus tests to obtain high-efficient active sites; weighting 1.0-2.0% of high-efficient active sites of fructus forsythiae essential oil, 2-3% of glycerol and 10-30% of Tween-80, mixing evenly, then slowly adding the mixture to balance water for injection, stirring evenly, standing at 1-4 DEG C for 2-5 days; and using millipore filters with the aperture of 0.45 mu m and 0.22 mu m to sequentially filter to obtain the nanoemulsion prepared from the high-efficient active sites of fructus forsythiae essential oil. Through the method, the pharmacological effects of essential oil is improved, the stimulation of fructus forsythiae essential oil is reduced, the activity of the essential oil is enhanced, and better therapeutic effect can be obtained through oral administration.
Description
Technical field
The present invention relates to a kind of method of from Forsythia volatile oil, isolating efficient disease-resistance pathogenic microorganism active site and being prepared into nano-emulsion, belong to medical technical field.
Background technology
Along with the globalization of economy, the globalization of information logistics, Ecological environment worsening in addition, pestilence are that the globalization of infectious disease also produces immediately.The generation of pestilence mainly is because the human infection pathogenic microorganism comprises antibacterial and virus with propagating, and therefore, mainly is exactly to utilize antibiotic and antiviral drugs for the treatment of infectious disease.At present, antibiotic on the market and antiviral drugs are that structure is clear, the single chemosynthesis of composition or semisynthetic drug, and it has played significant effect for the prevention and the treatment of infectious disease at the beginning of coming out really.But because the composition of chemicals is single, it is easy to be discerned by pathogenic microorganism and pathogenic microorganism is developed immunity to drugs, and the research and development that cause being used at present the new drug of infectious disease thus obviously lag behind the Drug resistance of pathogenic microorganism; Its toxic and side effects to human body that produces in therapeutic process also becomes increasingly conspicuous and is serious simultaneously, and for example the toxic and side effects of Tetracyclines, streptomycin class and aminoglycosides is well-known.Therefore, the medicine of the infectivity resistant disease of development of new highly effective and safe is extremely urgent.
Chinese medicine has the comprehensive function characteristics of multicomponent, many target spots, many effects, and significant broad-spectrum antiseptic, antivirus action are arranged, and its to human body nontoxic or toxicity and untoward reaction extremely low.Because its active component is complicated multicomponent, so antibacterial and virus are difficult for developing immunity to drugs for Chinese medicine, human body also is difficult for producing toleration.
The Fructus Forsythiae bitter in the mouth is slightly cold, and returns lung, the heart, small intestine meridian, has heat-clearing and toxic substances removing, the effect of dispersing swelling and dissipating binds, can be used for affection due to external wind and heat, pestilence from the beginning of.And modern study has remarkable inhibitory action for multiple virus, and its antiviral main active is a volatile oil.Forsythia volatile oil has the effect of broad-spectrum antiseptic anti-viral, and the influenza virus infecting mouse is had protective effect; The propagation that in Embryo Gallus domesticus, can suppress influenza virus A-prime, the strain of parainfluenza celestial platform.Wherein Forsythia volatile oil is 1: 65536 for the minimum antiviral concentration of influenza A virus (68-1 of capital section strain) and I type parainfluenza virus (celestial platform strain).
Volatile oil is a big class active ingredient of Chinese herbs.The complicated component of volatile oil, and structural similarity; Have pharmacological action widely such as antibiotic, antiviral and antiinflammatory action, but have certain zest, particularly oral zest is bigger.For a long time, not to the deep research of Forsythia volatile oil.The present invention is its high activity position of separation screening from Forsythia volatile oil, is prepared into nano-emulsion then, improves activity to reduce its zest.
Summary of the invention
The object of the present invention is to provide a kind of method of separating the high-efficiency activated position of Forsythia volatile oil and preparing nano-emulsion, this method has not only improved the activity of Forsythia volatile oil, has reduced its zest simultaneously.
Implementation procedure of the present invention is as follows:
The preparation method of the high-efficiency activated position of a kind of Forsythia volatile oil nano-emulsion may further comprise the steps:
(1) separation at the high-efficiency activated position of Forsythia volatile oil
Obtain Forsythia volatile oil different activities position by silica gel column chromatography or the separation of low pressure vacuum fractionation method, then the different activities position is obtained high-efficiency activated position by antibiotic or antivirus test screening;
(2) preparation of nano-emulsion
Take by weighing 1.0%～2.0% the high-efficiency activated position of Forsythia volatile oil, 2%～3% glycerol, 10%～30% tween 80 mix homogeneously, slowly join in the water for injection of surplus then, stir, placed 2～5 days for 1～4 ℃, microporous filter membrane with 0.45 μ m, 0.22 μ m filters successively, promptly gets the nano-emulsion at the high-efficiency activated position of Forsythia volatile oil.
The active site separation method of above-mentioned Forsythia volatile oil can have two kinds:
(1) silica gel column chromatography: varying in size according to polarity is separated into the different position of a plurality of polarity with Forsythia volatile oil, specifically be with Forsythia volatile oil sample on silicagel column, carry out eluting with organic solvent, the eluent that Fractional Collections is different, vacuum condition is removed organic solvent down, obtains the active site that polarity varies in size.
(2) low pressure vacuum fractionation method: separate by the boiling point difference, separate the different position of boiling point.Under the vacuum condition, the composition of different boiling is separated in rectifying column, condensation is collected and is obtained the different active site of boiling point.
The screening technique at the high activity position of above-mentioned Forsythia volatile oil filters out activity different parts preferably for the different parts that separation is obtained carries out antibiotic or antivirus test; Then different parts is optimized combination, carries out screening test again, thereby draw the highest active position.
The high activity position nano-emulsion of above-mentioned Forsythia volatile oil consist of Forsythia volatile oil 1.0%～2.0%, glycerol 2%～3%, tween 80 10%～30%, water for injection adds to 100%.
The present invention is its high activity position of separation screening from Forsythia volatile oil, be prepared into nano-emulsion then, not only improved the pharmacological action of volatile oil, also reduced the zest of Forsythia volatile oil and improve its activity, can obtain better therapeutic effect by oral administration.
The specific embodiment
Embodiment 1: silica gel column chromatography separates different parts
Adorn post with wet method, add in 200mL petroleum ether to the 70 gram silica gel, remove district's bubble, the dress post, last sample 1 gram Forsythia volatile oil adds petroleum ether respectively: ethyl acetate=15: 1; 13: 1; 11: 1; 9: 1; 7: 1; 5: 1; 3: 1; 1: 1; 1: 3; 1: 5 eluting, each eluent 200mL is in charge of and reclaims every pipe 10mL, and point sample is with the colour developing of sulphuric acid ethanol.Reclaim the roughly the same position of polarity, get final product.
Embodiment 2: low pressure vacuum fractionation method is separated different parts
2.1. tower is washed with dehydrated alcohol, open condensed water, under the state of normal pressure infinite reflux, washed tower 3 hours, with vacuum pump alcohol vapour in the tower is drained then.
2.2. measure an amount of Forsythia volatile oil, itself and zeolite added in the cleaned tower still in the lump; The sealing rectifying column also guarantees its seal; Opening vacuum pump control tower top pressure is-0.07MPa to begin to be heated to volatile oil and reach slight boiling condition (150 ℃～154 ℃).
Make thermograde heat up promptly 25 ℃～30 ℃ → 58 ℃～62 ℃ → 64 ℃～72 ℃ → 85 ℃～116 ℃ → 120 ℃～130 ℃ 2.3. adjust the rectifying column insulation instrument; Collecting under each temperature corresponding rectification position respectively is B1, B2, B3, B4, B5, B6.Note: the device parameter of rectifying column is: internal diameter is
Tower height 1000mm, in adorn 2.5 * 2.5mm θ glass cross filler, the filler loading height is about 900mm; Body of the tower adopts electric insulation belt heating, glass insulating layer and asbestos to unite insulation from inside to outside, and electric insulation belt heating power is controlled by pressure regulator, with the heat loss of compensation body of the tower.
Embodiment 3: different activities position bacteriostatic experiment
(1) activation of strain: tried strain (reference culture) and be inoculated in the solid agar culture medium, 37 ℃ of activation 24h, staphylococcus aureus activation 48h.
(2) preparation of bacteria suspension: after will activating tried strain with inoculating loop picking lawn in normal saline, make and contain bacterium and count turbidity to be about the bacteria suspension of 0.5Mcf standby.
(3) preparation of each active site solution: each tested each active site is dissolved in 1.0% HAc solution, and Forsythia volatile oil concentration is set to 2%, 1.5%, 1.0%, 0.5%, 0.25%.
(4) antibacterial method of testing (agar diffusion paper disk method)
Disk diffusion method is to be attached on the agar surface of having inoculated the test bacterium containing quantitative antibiotic filter paper, medicine in the scraps of paper spreads in agar, along with being logarithm, the antibiotic concentration of the increase of diffusion length reduces, in the scope that drug level arrives, can not grow and form transparent inhibition zone the antibacterial of this susceptibility sense, the inhibition zone that different bacterium forms has nothing in common with each other, and the size of inhibition zone has reflected the sensitivity of test bacterium to this medicine.If antibacterial can kill or suppress to supply in the ware growth of examination bacterium, inhibition zone the transparent circle of an asepsis growth then can appear, i.e. around filter paper.As deliberated index, antibacterial circle diameter is big more with the diameter of inhibition zone, illustrate that this antibacterial is good more for the inhibition effect of examination bacterium to this kind, otherwise it is poor more then to suppress effect.
Experiment is found: petroleum ether: ethyl acetate is the inhibition zone maximum of the active site of 15: 1～11: 1 eluting, reaches 26mm, illustrates that this position is the most concentrated position of active component.Promptly get the high-efficiency activated position of Forsythia volatile oil after removing organic solvent.
Embodiment 4: the preparation of nano-emulsion
Accurately measure the high-efficiency activated position 1.5ml of Forsythia volatile oil, glycerol 2.5ml, tween 80 12ml mix homogeneously; Slowly join in the 84ml water for injection then, stir; Placed 96 hours for 4 ℃, filter successively with the microporous filter membrane of 0.45 μ m, 0.22 μ m, promptly.
Claims (3)
1. the preparation method of the high-efficiency activated position of Forsythia volatile oil nano-emulsion is characterized in that may further comprise the steps:
(1) separation at the high-efficiency activated position of Forsythia volatile oil
Obtain Forsythia volatile oil different activities position by silica gel column chromatography or the separation of low pressure vacuum fractionation method, then the different activities position is obtained high-efficiency activated position by antibiotic or antivirus test screening;
(2) preparation of nano-emulsion
Take by weighing 1.0%～2.0% the high-efficiency activated position of Forsythia volatile oil, 2%～3% glycerol, 10%～30% tween 80 mix homogeneously, slowly join in the water for injection of surplus then, stir, placed 2～5 days for 1～4 ℃, microporous filter membrane with 0.45 μ m, 0.22 μ m filters successively, promptly gets the nano-emulsion at the high-efficiency activated position of Forsythia volatile oil.
2. according to the preparation method of the high-efficiency activated position of Forsythia volatile oil nano-emulsion, it is characterized in that: with Forsythia volatile oil sample on silicagel column, carry out eluting, the eluent that Fractional Collections is different with organic solvent, vacuum condition is removed organic solvent down, obtains the active site that polarity varies in size.
3. according to the preparation method of the high-efficiency activated position of Forsythia volatile oil nano-emulsion, it is characterized in that: under the vacuum condition, the composition of different boiling is separated in rectifying column, condensation is collected and is obtained the different active site of boiling point.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2959911A4 (en) * | 2013-06-12 | 2016-01-06 | Xiaoyan Zhang | Compound fructus forsythiae-radix bupleuri oil nanoemulsion preparation |
| CN109260151A (en) * | 2018-10-30 | 2019-01-25 | 成都中医药大学 | A kind of Forsythia volatile oil is from micro emulsion and preparation method thereof |
| CN110101659A (en) * | 2019-05-20 | 2019-08-09 | 山西大学 | A kind of phillygenol is from micro emulsion and preparation method thereof |
-
2010
- 2010-09-08 CN CN2010102752531A patent/CN101933976B/en not_active Expired - Fee Related
Non-Patent Citations (3)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库医药卫生科技辑》 20090815 李凡 连翘挥发油不同馏分药效学及自乳化给药系统的研究 第14-60页 1-3 , 第8期 2 * |
| 《中成药》 20081031 唐斌斌等 连翘萜烯脂肪乳制备工艺研究 第1458-1461页 1-3 第30卷, 第10期 2 * |
| 《青岛大学医学院学报》 20020630 严银芳等 石香薷挥发油抗流感病毒活性成分的初步研究 第155-157页 1-3 第38卷, 第2期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2959911A4 (en) * | 2013-06-12 | 2016-01-06 | Xiaoyan Zhang | Compound fructus forsythiae-radix bupleuri oil nanoemulsion preparation |
| CN109260151A (en) * | 2018-10-30 | 2019-01-25 | 成都中医药大学 | A kind of Forsythia volatile oil is from micro emulsion and preparation method thereof |
| CN109260151B (en) * | 2018-10-30 | 2021-03-19 | 成都中医药大学 | Forsythia volatile oil self-microemulsion and preparation method thereof |
| CN110101659A (en) * | 2019-05-20 | 2019-08-09 | 山西大学 | A kind of phillygenol is from micro emulsion and preparation method thereof |
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| CN101933976B (en) | 2012-10-31 |
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