CN101574093A - New preparation technology and new applications of syringa amurensis rupr bar volatile oil - Google Patents
New preparation technology and new applications of syringa amurensis rupr bar volatile oil Download PDFInfo
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Abstract
本发明所属医药产品研究开发技术领域。本发明涉及以暴马丁香(Syringa amurensis Rupr)树皮挥发油的制备新工艺和新用途。取暴马丁香树皮，干燥后剪碎，用蒸馏水浸泡12h后超声30min，温度为30℃，功率为80W。将药材与浸泡液一同倒入挥发油提取器中，采用水蒸汽蒸馏法提取3h。放出水层，用乙醚反复洗挥发油提取器，使暴马丁香挥发油充分溶解到乙醚中。将溶有挥发油的乙醚溶液倒入烧杯中，再向烧杯中加无水硫酸钠吸干水分，回收乙醚后即得到纯净的挥发油，放入冰箱4℃保存备用。本发明暴马丁香树皮挥发油对大肠杆菌、金黄色葡萄球菌、巴氏菌、链球菌、沙门氏菌均有不同程度的抑制作用，可开发为天然抗菌剂应用于食品、药品等行业，制备出具有抑菌作用的各种形式的产品。The invention belongs to the technical field of research and development of pharmaceutical products. The invention relates to a new preparation process and a new application of the volatile oil from the bark of Syringa amurensis Rupr. Take the bark of the bark of Cinnamomum chinensis, cut it into pieces after drying, soak it in distilled water for 12 hours, and then sonicate it for 30 minutes at a temperature of 30°C and a power of 80W. Pour the medicinal materials together with the soaking liquid into a volatile oil extractor, and extract by steam distillation for 3 hours. Release the water layer, and repeatedly wash the volatile oil extractor with ether to fully dissolve the volatile oil of Matinaceae in ether. Pour the diethyl ether solution in which the volatile oil is dissolved into a beaker, then add anhydrous sodium sulfate to the beaker to absorb the water, recover the diethyl ether to obtain pure volatile oil, and store it in the refrigerator at 4°C for later use. The bark volatile oil of the present invention has different degrees of inhibitory effects on Escherichia coli, Staphylococcus aureus, Pasteurella, Streptococcus and Salmonella, and can be developed as a natural antibacterial agent and applied to industries such as food and medicine to prepare a product with Bacteriostatic effect of various forms of products.
Description
Technical field
Medical product research and development technical field under the present invention.The present invention relates to new preparation process and new purposes with syringa reticulata var mandshurica Syringa amurensis Rupr. bark volatile oil.
Background technology
Syringa reticulata var mandshurica Syringa amurensis Rupr. is one of common medicinal plant in Changbai Mountain, mainly is distributed in Jilin, Liaoning, North China, northwest and Central China, aboundresources in China.Bark, trunk and branch are all pharmaceutically acceptable, bitter, cold nature, experimental results show that through modern pharmacology have lung heat clearing away, sputum eliminating, cough-relieving, relieving asthma, the function of anti-inflammatory, diuresis.
At present,, only there are several pieces of reports from bark, branch, to separate and obtain several compounds, the syringa reticulata var mandshurica bark volatile oil was not done antibacterial research about syringa reticulata var mandshurica bark volatile oil and chemical composition and the rarely seen report of pharmacological research.Therefore, the present invention adopts the syringa reticulata var mandshurica bark, shreds after the drying, and with ultrasonic 30min behind the distilled water immersion 12h, temperature is 30 ℃, and power is 80W.Medicinal material and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 3h.Emit water layer, wash volatile oil extractor repeatedly, syringa reticulata var mandshurica volatile oil fully is dissolved in the ether with ether.The diethyl ether solution that is dissolved with volatile oil is poured in the beaker, added the anhydrous sodium sulfate suck dry moisture again in beaker, promptly obtain pure volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
Syringa reticulata var mandshurica bark volatile oil of the present invention is inhibited to gram-positive bacteria, Gram-negative bacteria, and this bacteriostasis has positive application in practice and is worth.Such as streptococcus is had good inhibition effect, diseases such as treatment purulent inflammation, scarlet fever, rheumatic fever, acute glomerulonephritis there is positive practice significance; Escherichia coli, staphylococcus aureus, salmonella there are good inhibition effect, prevention and treatment food posioning are had positive role.This is for enlarging syringa reticulata var mandshurica medicine source, and it is significant that it is carried out rational exploitation and utilization.
Summary of the invention
The purpose of this invention is to provide a kind of new preparation process of the syringa reticulata var mandshurica bark volatile oil with bacteriostatic activity and the syringa reticulata var mandshurica bark volatile oil is developed and applied in having the product of bacteriostasis.
1. be the new technology and the new purposes of feedstock production volatile oil with the syringa reticulata var mandshurica bark, and the syringa reticulata var mandshurica bark volatile oil is developed and applied in having the product of bacteriostasis.
Syringa reticulata var mandshurica bark volatile oil of the present invention all has inhibitory action in various degree to Escherichia coli, staphylococcus aureus, Pasteur bacterium, streptococcus, salmonella, can be developed as natural antibacterial agent and be applied to industries such as food, medicine, prepare various forms of products with bacteriostasis.
2. new technology for preparing the syringa reticulata var mandshurica bark volatile oil is characterized in that this technology comprises following process:
(1) get the syringa reticulata var mandshurica bark, choose the impurity elimination thing, washing is dried or is dried, and pulverizes, and with ultrasonic 30min behind the distilled water immersion 12h, temperature is that 30 ℃ of power are 80W;
(2) (1) traditional Chinese medicine and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 3h, the floating aqueous solution that volatile oil is arranged above obtaining;
(3) there is the aqueous solution of volatile oil to emit water layer top floating in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain pure volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
3. the raw material of 1 to 2 described preparation syringa reticulata var mandshurica bark volatile oil is the bark of syringa reticulata var mandshurica Syringaamurensis Rupr. according to the present invention.
4. 1 to 2 described syringa reticulata var mandshurica bark volatile oil all has inhibitory action in various degree to Escherichia coli, staphylococcus aureus, Pasteur bacterium, streptococcus, salmonella according to the present invention.
5. 1 to the 2 described syringa reticulata var mandshurica bark volatile oil according to the present invention is characterized in that this bark volatile oil can be used as natural antibacterial agent and is used for industries such as food, medicine, replaces the synthetic antibacterial agents of toxic side effect.
6. according to the present invention, " % " among the present invention is percentage by weight.
Embodiment
Syringa reticulata var mandshurica bark volatile oil new preparation process of the present invention comprises following examples, and the following examples can further specify the present invention, but do not limit the present invention in any way.
Embodiment 1:
(1) get syringa reticulata var mandshurica bark 100g, choose the impurity elimination thing, washing is dried or is dried, and pulverizes, and with ultrasonic 30min behind the 400mL distilled water immersion 12h, temperature is that 30 ℃ of power are 80W;
(2) (1) traditional Chinese medicine and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 3h, the floating aqueous solution that volatile oil is arranged above obtaining;
(3) there is the aqueous solution of volatile oil to emit water layer top floating in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain pure volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
Embodiment 2:
(1) get syringa reticulata var mandshurica bark 200g, choose the impurity elimination thing, washing is dried or is dried, and pulverizes, and with ultrasonic 30min behind the 600mL distilled water immersion 12h, temperature is that 30 ℃ of power are 80W;
(2) (1) traditional Chinese medicine and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 3h, the floating aqueous solution that volatile oil is arranged above obtaining;
(3) there is the aqueous solution of volatile oil to emit water layer top floating in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain pure volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
Pharmacological test example: the bacteriostasis of syringa reticulata var mandshurica bark volatile oil
1 experiment material
Escherichia coli, streptococcus, salmonella, Pasteur bacterium and staphylococcus aureus all come from Jilin Agriculture University Preventive Veterinary Medicine laboratory, cultivate 12h for 37 ℃ in the peptone steamed beef soup.
Medium is a beef-protein medium.Use liquid nutrient medium when activation of bacterium and cultivation, consist of: beef extract: peptone: sodium chloride: distilled water (3: 10: 5: 1000).Use solid culture medium when preservation of bacterium and bacteriostatic experiment, consist of: beef extract: peptone: sodium chloride: agar: distilled water (3: 10: 5: 22: 1000).
2 experimental techniques
2.1 culture medium preparation
Get beef extract 0.6g, peptone 2g, sodium chloride 1g, distilled water 200ml, mix and stir that it is dissolved fully, be made into liquid nutrient medium.Measure liquid nutrient medium with graduated cylinder, its average mark is contained in the triangular flask of 10 50ml every bottle of 20ml.Get beef extract 3g, peptone 10g, sodium chloride 5g, agar 22g, distilled water 1000ml, be placed on the Electric stove after the mixing and heat, agar is dissolved fully, be made into solid culture medium.Measure solid culture medium with graduated cylinder, its average mark is contained in the triangular flask of 5 150ml every bottle of 100ml.The triangular flask bottleneck is all wrapped up with the tampon jam-pack and with brown paper.
2.2 sterilization
The solid culture medium, the liquid nutrient medium that prepare are all put into high-pressure sterilizing pot and sterilized, and when temperature rose to 121 ℃, 20min picked up counting.Experiment equipments such as culture dish, graduated cylinder, tweezers, scissors, 6mm filter paper (being placed in the small beaker), dropper, ampoule bottle are all put into 170 ℃ of sterilizations of baking oven 2h.Experiment is preceding with 75% ethanol wiping superclean bench and ultraviolet sterilization 20min.37 ℃ of constant incubators need be sterilized with 75% ethanol wiping before use.
2.3 the cultivation of bacterium with look into bacterium
5 bacterial classifications are poured in the triangular flask that liquid nutrient medium is housed on superclean bench, under the alcolhol burner environment, and every kind of bacterium is cultivated two parts.These 10 triangular flasks are put into shaking table shake bacterium 6h for 37 ℃.Microscope begins to look into bacterium after doing microscopy, and record data also calculate bacteria concentration, if 5 medium square total bacteria counts are A, bacterium liquid extension rate is B, then total bacteria count=A/5 * 25 * 10000 * 13=50000AB in the 1ml bacterium liquid
2.4 the preparation of sample liquid and filter paper
The syringa reticulata var mandshurica bark volatile oil is mixed with the solution (can add 0～4 μ L dimethyl sulfoxide (DMSO) hydrotropy) of 5mg/ml, by 1: 2
nBe diluted to the solution of 2.5mg/ml, 1.25mg/ml, 0.625mg/ml, 0.3125mg/ml.Filter paper is broken into the disk that diameter is 6mm with card punch, at superclean bench filter paper is put in each gradient sample and soaked 2h.
2.5 the preparation of bacterio-agar flat board is arranged
The bacterium liquid that dilution is good mixes with solid culture medium and rocks evenly, and this moment, the concentration of bacterium should reach 3.6 * 10
8CFU/ml.To there be bacterium culture medium to pour into successively in each culture dish, and rock culture dish and make medium be layered on the culture dish bottom equably, and be cooled to and solidify.
2.6 bacteriostatic experiment method
, in that label on the bacterio-agar flat board is arranged soaked filter paper is pressed from both sides out with tweezers with marking pen, puts into the culture dish of writing corresponding contrast numbering, each sample do three parallel, put into 37 ℃ of constant incubators and cultivate.
3. experimental result
3.1 fungistatic effect is represented (mm of unit) with antibacterial circle diameter DD
12h, 24h after bacteriostatic experiment finishes, 36h, 48h observe the growing state of bacterium, measure antibacterial circle diameter and record.
The bacteriostatic activity of table 1 syringa reticulata var mandshurica bark volatile oil
3.2 the mensuration of minimal inhibitory concentration MIC (mg/ml of unit)
Water is cooked negative control, and streptomycin is done positive control, and the fungistatic effect of volatile oil and the two contrast draw minimal inhibitory concentration.
The minimal inhibitory concentration MIC of table 2 syringa reticulata var mandshurica bark volatile oil (mg/ml of unit)
The result shows: the syringa reticulata var mandshurica bark volatile oil all has inhibitory action in various degree to Escherichia coli, streptococcus, salmonella, Pasteur bacterium, staphylococcus aureus.Volatile oil to the minimal inhibitory concentrations of five kinds of bacterium between 0.63mg/ml～5.00mg/ml.
Fine by concrete embodiment explanation syringa reticulata var mandshurica bark volatile oil fungistatic effect, can be used as natural antibacterial agent and be used for industries such as food, medicine, replace the synthetic antibacterial agents of toxic side effect.Syringa reticulata var mandshurica volatile oil has good inhibition effect to streptococcus, can prepare the medicine of various formulations, is used for the treatment of diseases such as purulent inflammation, scarlet fever, rheumatic fever, acute glomerulonephritis.Escherichia coli, staphylococcus aureus, salmonella there is good inhibition effect; The medicine that can prepare food additives and various formulations is used to prevent and treat the food poisoning that is caused by germ contamination because of food.
Syringa reticulata var mandshurica is in the history of cultivating of existing 1000 of China, and aboundresources is drawn materials conveniently, is fit to large scale investment production, has increased the feasibility of exploitation, has important practice significance and DEVELOPMENT PROSPECT.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845737A (en) * | 2014-02-17 | 2015-08-19 | 天士力制药集团股份有限公司 | Extraction method for volatile oil in radix bupleuri |
| CN106106571A (en) * | 2016-06-23 | 2016-11-16 | 袁春华 | A kind of method utilizing Gourmet Powder Factory's waste liquid compound botanical oil to prepare disinfectant use in agriculture |
| CN106221934A (en) * | 2016-08-26 | 2016-12-14 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Fructus Amomi Rotundus quintessence oil |
| CN110305730A (en) * | 2019-05-28 | 2019-10-08 | 苏州科技大学 | Extraction technology and application of volatile oil from Changshu white celery |
| CN110613787A (en) * | 2019-10-29 | 2019-12-27 | 张少清 | Vegetable oil composition and preparation method and application thereof |
-
2009
- 2009-06-22 CN CNA2009100671467A patent/CN101574093A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845737A (en) * | 2014-02-17 | 2015-08-19 | 天士力制药集团股份有限公司 | Extraction method for volatile oil in radix bupleuri |
| CN104845737B (en) * | 2014-02-17 | 2020-03-17 | 天士力医药集团股份有限公司 | Method for extracting volatile oil from radix bupleuri |
| CN106106571A (en) * | 2016-06-23 | 2016-11-16 | 袁春华 | A kind of method utilizing Gourmet Powder Factory's waste liquid compound botanical oil to prepare disinfectant use in agriculture |
| CN106221934A (en) * | 2016-08-26 | 2016-12-14 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Fructus Amomi Rotundus quintessence oil |
| CN110305730A (en) * | 2019-05-28 | 2019-10-08 | 苏州科技大学 | Extraction technology and application of volatile oil from Changshu white celery |
| CN110613787A (en) * | 2019-10-29 | 2019-12-27 | 张少清 | Vegetable oil composition and preparation method and application thereof |
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Application publication date: 20091111 |