CN102250174A - Method for extracting jasminin from winter jasmine leaves - Google Patents
Method for extracting jasminin from winter jasmine leaves Download PDFInfo
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- CN102250174A CN102250174A CN2011102088009A CN201110208800A CN102250174A CN 102250174 A CN102250174 A CN 102250174A CN 2011102088009 A CN2011102088009 A CN 2011102088009A CN 201110208800 A CN201110208800 A CN 201110208800A CN 102250174 A CN102250174 A CN 102250174A
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Abstract
The invention relates to a method for extracting and purifying jasminin from winter jasmine leaves, belonging to the technical field of plant extracts. The jasminin is extracted and purified from winter jasmine leaves through solvent extraction, filtration, filtrate concentration, solvent extraction, silica gel column chromatography, eluent concentration, crystallization and other methods. The method is convenient and easy to operate and control, and has the advantages of short production cycle, low production cost, reutilization of extraction solvent and the like. The purified substance is identified as the jasminin through physical and chemical inspection and spectral analysis data authentication; and the monomer has high antimicrobial activity, and can be used as an antimicrobial preparation material or antimicrobial lead compound for deep development, utilization and research.
Description
Technical field
The present invention relates to effective ingredients in plant extraction process field, be specifically related to a kind of Leaf of Winter Jasmine active compound monomer extraction process that bacteriostatic action is arranged.
Background technology
Winter Jasmine (
Jasminum nudiflorumLindl.) chain timbers Rhinocerotidae Flower of Arabian Jasmine platymiscium, its vitality is extremely strong, and early spring, the cold spell in spring material string that promptly bursts forth in pretty was gone here and there golden yellow flower, and for the afforestation of Chinese elite beautifies kind, extensively there is cultivation each region, the Yangtze valley.State Winter Jasmine in the Compendium of Material Medica and control pyogenic infections evil sore, it also is western Hunan herbal medicine commonly used among the people, its leaf hardship, puckery, flat, nontoxic, can detoxify heat-clearing, hemostasis, pain relieving are used for the treatment of diseases such as wound, traumatic hemorrhage, stomatitis, gynecological inflammation, carbuncle furuncle poison and vulva pruritus.Spend and often make tea-drinking, its flavor is sweet, puckery, flat, clearing away heat and promoting diuresis, detoxifcation, can treat have a headache and fever, urinary system infection and the ulcer of lower limb.Branch, the leaf of document record Winter Jasmine contain syringoside (Syringin), jasmiflorin (Jasmiflorin) and jasmipicrin (Jasmipierin).The report of external existing Leaf of Winter Jasmine chemical composition, but the biological activity of Winter Jasmine chemical composition and the research of actives extraction separation thereof are not appeared in the newspapers as yet, the applicant has detected the bacteriostatic activity of Leaf of Winter Jasmine and actives has been carried out extraction separation research for this reason, from Leaf of Winter Jasmine, be separated to the monomer of the strong bacteriostatic activity of a tool, through physics and chemistry detection and HPLC, IR,
1H-NMR,
13Spectral data analysis confirmations such as C-NMR, EI-MS, DEPT are the winter jasmine florigen.Known winter jasmine florigen structure is as follows:
On this research basis, repeat, improve, enlarge experiment, obtain the winter jasmine florigen and extract the purifying new technology.
Summary of the invention
The invention provides a kind of method of extracting high-purity winter jasmine florigen (jasminin) from Leaf of Winter Jasmine, this method is easy and simple to handle, with short production cycle, with low cost, be easy to carry out industrialization production.
Embodiment of the present invention are: a kind of method of extracting the winter jasmine florigen from Leaf of Winter Jasmine may further comprise the steps:
(1) 45 ℃ of oven dry of Leaf of Winter Jasmine are pulverized, and cross 40 mesh sieves, add 80% ~ 90% ethanolic soln lixiviate 3 times, and 50～60 ℃ of extraction temperatures are collected extracting solution, and vacuum concentration reclaims concentrated solution;
(2) again with ethyl acetate normal temperature extraction 3～5 times, the extraction time is 2h to concentrated solution at every turn with sherwood oil normal temperature extraction 3～5 times, gained water;
(3) collect ethyl acetate phase extract, vacuum concentration;
(4) enriched material is carried out silica gel column chromatography, the chloroform-methanol solvent gradient elution is collected elutriant and is concentrated;
(5) enriched material dissolve with ethanol, crystallization, drying obtains white crystalline compound, is target compound.
In the step (1), 3 times extraction time is respectively 2h, 1h, 1h, and each feed liquid mass volume ratio is 1g:6～8ml.The lixiviate optimum temperuture is 60 ℃.
In the step (3), thickening temperature is 50～60 ℃.
In the step (4), during the chloroform-methanol gradient elution, the volume ratio of chloroform and methyl alcohol is respectively 2:1,3:1,4:1, and the gained elutriant concentrated when collection chloroform and methyl alcohol volume ratio were 3:1.
Product of the present invention is winter jasmine florigen, purity 〉=95% through the HPLC analysis confirmation.Product detects through dull and stereotyped paper disk method, test tube method has stronger bacteriostatic activity.Product of the present invention can be used for preparing antibiotic preparation, raw material or antibiotic lead compound and carries out the research that deep development utilizes.
Innovative point of the present invention is as follows: the series methods technology that (1) the present invention adopts is comparatively easy, be easy to control, with short production cycle, production cost is low; (2) the winter jasmine florigen of the present invention's extraction is analyzed through HPLC, and purity 〉=95% has higher bacteriostatic activity; (3) extract the recyclable utilization of solvent material, environmental pollution is very little.
Specific embodiments
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto.
The yield of product described in following examples account form is:
Product yield (%)=quality product/Leaf of Winter Jasmine raw materials quality * 100.
Florigen high performance liquid chromatography (HPLC) testing conditions of welcoming spring in the product described in following examples is: chromatographic column Waters YWG C
18(5 μ m, 3.9mm * 150mm); Moving phase: second eyeball: water=30:70; Column temperature is a room temperature; Detect wavelength: 240nm; Sample size 10 μ l; Flow velocity 1.0ml/min.
Embodiment 1:
With 250g Leaf of Winter Jasmine powder, add 80% ethanol 2000ml, 60 ℃ of lixiviate 2h, suction filtration are got filter residue and are added 80% ethanol 1000ml and extract for the 2nd time, 60 ℃ of 1h, suction filtration, get filter residue and add the 3rd extraction of 80% ethanol 1000ml, 60 ℃ of 1h, suction filtration merge 3 times filtrate, concentrate, thickening temperature≤55 ℃ are concentrated into no ethanol.Add equivalent petroleum ether extraction 3-5 time in the concentrated solution, take off a layer water, add the equivalent ethyl acetate extraction, repeat 3-5 time, the combined ethyl acetate extraction liquid, Rotary Evaporators concentrates.Enriched material carries out silica gel column chromatography, and the chloroform-methanol gradient elution is collected elutriant and concentrated.Enriched material adds 90% ethanol crystallization.The white crystal 3.15g that recrystallization obtains for 2-3 time.The product yield is 1.26%, and detecting the Winter Jasmine cellulose content through HPLC is 98.06%.
Embodiment 2
Leaf of Winter Jasmine powder 250g adds 85% ethanol 2000ml, 60 ℃ of lixiviate 2h, suction filtration, get filter residue and add the 2nd extraction of 85% ethanol 1000ml, 60 ℃, 1h, suction filtration, filter residue adds 85% ethanol 1000ml and extracts for the 3rd time, 70 ℃ of 1h, suction filtration merge 3 times filtrate, concentrate, thickening temperature≤55 ℃ are concentrated into no ethanol.Enriched material adds the equivalent petroleum ether extraction 5 times, takes off a layer water, adds the equivalent ethyl acetate extraction, repeat 5 times, and the combined ethyl acetate extraction liquid, Rotary Evaporators is concentrated into dry powdered.Enriched material carries out silica gel column chromatography, and the chloroform-methanol gradient elution is collected elutriant and concentrated.Enriched material adds 90% ethanol crystallization.The white crystal 3.4g that recrystallization obtains for 2-3 time, the product yield is 1.36%, detecting the Winter Jasmine cellulose content through HPLC is 99.17%.
Embodiment 3
Leaf of Winter Jasmine powder 250g adds 90% ethanol 2000ml, 60 ℃ of lixiviate 2h, suction filtration, get filter residue and add the 2nd extraction of 90% ethanol 1000ml, 60 ℃ of 1h, suction filtration, filter residue adds 90% ethanol 1000ml the 3rd time and extracts, and 60 ℃ of 1h, suction filtration merge 3 times filtrate, concentrate, thickening temperature≤55 ℃ are concentrated into no ethanol, enriched material adds the extracting 3 times of sherwood oil of equivalent, takes off a layer water, adds the equivalent ethyl acetate extraction, repeat 3 times, the combined ethyl acetate extraction liquid, Rotary Evaporators concentrates.The enriched material silica gel column chromatography, the chloroform-methanol gradient elution is collected elutriant and is concentrated.Enriched material adds 90% ethanol crystallization.The white crystal 3.3g that recrystallization obtains for 2-3 time, the product yield is 1.32%, detecting the Winter Jasmine cellulose content through HPLC is 98.62%.
Claims (5)
1. a method of extracting the winter jasmine florigen from Leaf of Winter Jasmine is characterized in that, may further comprise the steps:
(1) 45 ℃ of oven dry of Leaf of Winter Jasmine are pulverized, and cross 40 mesh sieves, add 80% ~ 90% ethanolic soln lixiviate 3 times, and 50～60 ℃ of extraction temperatures are collected extracting solution, and vacuum concentration reclaims concentrated solution;
(2) concentrated solution extracts 3～5 times with sherwood oil normal temperature, and with ethyl acetate normal temperature extraction 3～5 times, the extraction time is 2h to the gained water at every turn again;
(3) collect ethyl acetate phase extract, vacuum concentration;
(4) enriched material is carried out silica gel column chromatography, the chloroform-methanol solvent gradient elution is collected elutriant and is concentrated;
(5) enriched material dissolve with ethanol, crystallization, drying obtains white crystalline compound, is target compound.
2. the method for extracting the winter jasmine florigen from Leaf of Winter Jasmine according to claim 1 is characterized in that in the step (1), 3 times extraction time is respectively 2h, 1h, 1h, and each feed liquid mass volume ratio is 1g:6～8ml.
3. the method for extracting the winter jasmine florigen from Leaf of Winter Jasmine according to claim 1 and 2 is characterized in that extraction temperature is 60 ℃.
4. the method for extracting the winter jasmine florigen from Leaf of Winter Jasmine according to claim 1 is characterized in that in the step (3), thickening temperature is 50～60 ℃.
5. the method for from Leaf of Winter Jasmine, extracting the winter jasmine florigen according to claim 1, it is characterized in that, in the step (4), during the chloroform-methanol gradient elution, the volume ratio of chloroform and methyl alcohol is respectively 2:1,2.5:1,3:1, and the gained elutriant concentrated when collection chloroform and methyl alcohol volume ratio were 3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011102088009A CN102250174A (en) | 2011-07-25 | 2011-07-25 | Method for extracting jasminin from winter jasmine leaves |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102088009A CN102250174A (en) | 2011-07-25 | 2011-07-25 | Method for extracting jasminin from winter jasmine leaves |
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| CN102250174A true CN102250174A (en) | 2011-11-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831546A (en) * | 2016-03-22 | 2016-08-10 | 张利文 | Winter jasmine extract and application thereof in preparation of food preservative |
| CN105963245A (en) * | 2016-04-22 | 2016-09-28 | 深圳大学 | Preparation method and application of jasminin solution |
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN111775249A (en) * | 2020-07-08 | 2020-10-16 | 安徽昌发实业有限公司 | Mildew-proof and corrosion-proof treatment method for rubber wood |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0418006A (en) * | 1990-05-09 | 1992-01-22 | Osaka Gas Co Ltd | Extraction and isolation of natural jasmine acid |
-
2011
- 2011-07-25 CN CN2011102088009A patent/CN102250174A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0418006A (en) * | 1990-05-09 | 1992-01-22 | Osaka Gas Co Ltd | Extraction and isolation of natural jasmine acid |
Non-Patent Citations (2)
| Title |
|---|
| 卢成瑛,等: "迎春花叶抑菌活性物研究", 《食品科学》 * |
| 杨政水: "迎春花色素的提取及稳定性研究", 《食品科技》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831546A (en) * | 2016-03-22 | 2016-08-10 | 张利文 | Winter jasmine extract and application thereof in preparation of food preservative |
| CN105963245A (en) * | 2016-04-22 | 2016-09-28 | 深圳大学 | Preparation method and application of jasminin solution |
| CN105963245B (en) * | 2016-04-22 | 2019-03-08 | 深圳大学 | A kind of preparation method and application of jasminin solution |
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN111775249A (en) * | 2020-07-08 | 2020-10-16 | 安徽昌发实业有限公司 | Mildew-proof and corrosion-proof treatment method for rubber wood |
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Application publication date: 20111123 |