CN103952240B - A kind of preparation method of Flower of Sunset Abelmoschus volatile oil - Google Patents
A kind of preparation method of Flower of Sunset Abelmoschus volatile oil Download PDFInfo
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- CN103952240B CN103952240B CN201410212474.2A CN201410212474A CN103952240B CN 103952240 B CN103952240 B CN 103952240B CN 201410212474 A CN201410212474 A CN 201410212474A CN 103952240 B CN103952240 B CN 103952240B
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Abstract
The present invention relates to a kind of volatile oil extractive technique field, specifically a kind of preparation method of Flower of Sunset Abelmoschus volatile oil.The Flower of Sunset Abelmoschus dried in the shade is pulverized in powdery; With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in extractor, add low boiling point solvent, it is colourless that reflux is extracted into solvent repeatedly, cooling, collection extracting solution; Most solvent is waved by concentrated for extracting solution; Loaded in extractor by the Flos abelmoschi manihot extract waving most solvent, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in extractor no longer to be increased, and cools, collects oil reservoir; In oil reservoir, add inorganic salt desiccant dehydration, sealing is preserved, and obtains Flower of Sunset Abelmoschus volatile oil.Owing to first heating continuous circumfluence extraction with low boiling point organic solvent, avoid the material interference such as glue class, phlegmatic temperament, polysaccharide.By extract distilling with water, then eliminate non-volatile impurities.Before distillation, low temperature flings to organic solvent, avoids the residual of solvent.
Description
Technical field
The present invention relates to a kind of volatile oil extractive technique field, specifically a kind of preparation method of Flower of Sunset Abelmoschus volatile oil.
Background technology
Flower of Sunset Abelmoschus is the dry corolla of Malvaceae plant Abelmoschus manihot (L.) Medic..2010 editions " Chinese Pharmacopoeias " record, and have damp-excreting medicinal clearly, and subduing swelling and detoxicating effect is held back for damp and hot heap soil or fertilizer over and around the roots, stranguria with turbid discharge oedema; Control swollen ulcer drug outward, burn due to hot liquid or fire etc.Song dynasty " good help book on Chinese herbal medicine ": control urine leaching and expedite the emergence of, main all evil sore pus are not recovered person for a long time again, do end and apply.Ming Dynasty's Compendium of Material Medica: subduing inflammation, immersion oil is coated with burn.At present extensive artificial culture, more to flavonoid in Flower of Sunset Abelmoschus, polysaccharose substance research, study less to contained volatile oil in spending.
The extracting method of volatile oil has a variety of, mainly contains steam distillation, solvent-extraction process, supercritical fluid extraction etc.Because Flower of Sunset Abelmoschus contains a large amount of Sunset Abelmoschus Root glue, phlegmatic temperament, polysaccharide etc., chance water then stripping makes solution thickness, and heating is easily charred, and affects the extraction of volatile oil; Be used alone solvent-extraction process, then containing a large amount of impurity such as resin, grease, wax, chlorophyll.
At present research is extracted seldom to fragrant volatile oil contained in Flower of Sunset Abelmoschus.Only have in the recent period one section (Zhang Yuanyuan, Jia Xiaoni, Cao Yongxiang, etc.Flower of Sunset Abelmoschus chemical constitution study [J], northwest pharmaceutical journal, 2008,23 (2): 80-82) what adopt is wet distillation, but find through actual verification, after Flower of Sunset Abelmoschus meets water, tackiness increases, and heat is just black a little.
Summary of the invention
In order to overcome the shortcoming part existed in above-mentioned prior art, the technical problem to be solved in the present invention is to provide a kind of preparation method of Flower of Sunset Abelmoschus volatile oil.
To achieve these goals, the technical solution adopted in the present invention is: a kind of preparation method of Flower of Sunset Abelmoschus volatile oil, and step is as follows:
1), the Flower of Sunset Abelmoschus dried in the shade is pulverized in powdery;
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in extractor, add low boiling point solvent, it is colourless that 40 ~ 60 DEG C of reflux are extracted into solvent repeatedly, cooling, collection extracting solution;
3) concentrate at, extracting solution being placed in 20 ~ 40 DEG C and wave most solvent;
4), distilling with water
Loaded in extractor by the Flos abelmoschi manihot extract waving most solvent, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in extractor no longer to be increased, and cools, collects oil reservoir;
5), in oil reservoir add inorganic salt desiccant dehydration, sealing is preserved, and obtains Flower of Sunset Abelmoschus volatile oil.
Preferably, described step 1) in the fineness of powdery Flower of Sunset Abelmoschus be 10 ~ 80 orders.
Preferably, described step 2) in extractor be apparatus,Soxhlet's.
Preferably, described step 2) in low boiling point solvent be ether.
Preferably, described step 4) in extractor be volatile oil extractor.
Preferably, described step 5) in inorganic salt siccative be anhydrous sodium sulphate.
The preparation method of Flower of Sunset Abelmoschus volatile oil of the present invention, its beneficial effect is embodied in:
1), the present invention contains a large amount of phlegmatic temperament, colloid etc. according to Flower of Sunset Abelmoschus, have the advantages that to meet the stripping of glue viscous substance, adopt and first use low boiling point organic solvent continuous circumfluence extraction, extract prepares Flower of Sunset Abelmoschus volatile oil by distilling with water method again.Meanwhile, owing to first heating continuous circumfluence extraction with low boiling point organic solvent, avoid the interference of the material such as glue class, phlegmatic temperament, polysaccharide, extract adds water distillation again, to eliminate involatile constituent.Through gas chromatography combined with mass spectrometry (GC-MS), first identified goes out in Flower of Sunset Abelmoschus volatile oil main containing aromatoising substance and active substances such as β-Se Lin alkene, camphor, borneol.
2), the invention solves the problem that Flower of Sunset Abelmoschus can not use water extraction volatile oil, Flower of Sunset Abelmoschus contains a large amount of Sunset Abelmoschus Root glue, phlegmatic temperament, polysaccharide etc., and chance water then stripping makes solution thickness, affects the extraction of volatile oil, and heating is easily charred.Meanwhile, if be used alone solvent-extraction process, easily containing a large amount of impurity such as resin, grease, wax, chlorophyll.The present invention by extract distilling with water, then eliminates non-volatile impurities.Before distillation, low temperature flings to organic solvent, avoids the residual of solvent.
3), whole leaching process temperature is not high, and heat-up time is short, avoids thermo-labile component in volatile oil and to be decomposed destruction.
4), mostly volatile oil is small-molecule substance, can be absorbed fast by body, effect extensively, cardio-cerebrovascular, central nervous system, respiratory system, gastrointestinal system, antibacterial, anti-inflammatory, anticancer, antiviral, promote that the many-sides such as drug absorption all have effect.The invention solves current Flower of Sunset Abelmoschus volatile oil and extract the defect existed, be the further investigation of Flower of Sunset Abelmoschus volatile oil, disclose its mechanism of action, Application and Development etc. are laid a good foundation.
Accompanying drawing explanation
Fig. 1 is the GC-MS total ion current figure of Flower of Sunset Abelmoschus volatile oil prepared by the embodiment of the present invention.
In figure:
1. camphor 2. borneol
3. β-Se Lin alkene 4.10s, 11s-Himachala-3 (12) 4-diene
5. trans-long pinocarveol 6. dibutyl phthalate
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but the present invention is not limited only to embodiment, and under the prerequisite not departing from present inventive concept, any improvement done all drops within protection scope of the present invention.
The preparation method of Flower of Sunset Abelmoschus volatile oil, step is as follows:
1), the Flower of Sunset Abelmoschus dried in the shade being crushed to fineness is 10 ~ 80 object powderies.
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in apparatus,Soxhlet's, add ether, it is colourless that 40 ~ 60 DEG C of reflux are extracted into solvent repeatedly, cooling, collection extracting solution.
3) concentrate at, extracting solution being placed in 20 ~ 40 DEG C and wave most solvent.
4), distilling with water
Loaded in volatile oil extractor by the Flos abelmoschi manihot extract waving most solvent, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in volatile oil extractor no longer to be increased, and cools, collects oil reservoir.
5), in oil reservoir add anhydrous sodium sulfate dehydration, sealing is preserved, and obtains the Flower of Sunset Abelmoschus volatile oil as shown in Fig. 1 collection of illustrative plates.
Above content is only to structure example of the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the structure of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (6)
1. a preparation method for Flower of Sunset Abelmoschus volatile oil, is characterized in that step is as follows:
1), the Flower of Sunset Abelmoschus dried in the shade is pulverized in powdery;
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in extractor, add low boiling point solvent, it is colourless that 40 ~ 60 DEG C of reflux are extracted into solvent repeatedly, cooling, collection extracting solution;
3) concentrate at, extracting solution being placed in 20 ~ 40 DEG C and wave most solvent;
4), distilling with water
Loaded in extractor by the Flos abelmoschi manihot extract waving most solvent, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in extractor no longer to be increased, and cools, collects oil reservoir;
5), in oil reservoir add inorganic salt desiccant dehydration, sealing is preserved, and obtains Flower of Sunset Abelmoschus volatile oil.
2. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 1) in the fineness of powdery Flower of Sunset Abelmoschus be 10 ~ 80 orders.
3. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 2) in extractor be apparatus,Soxhlet's.
4. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 2) in low boiling point solvent be ether.
5. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 4) in extractor be volatile oil extractor.
6. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 5) in inorganic salt siccative be anhydrous sodium sulphate.
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CN107629874A (en) * | 2017-10-10 | 2018-01-26 | 广东长利香精香料有限公司 | A kind of cinnamomum camphora Verbena officinalis essential oil |
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CN105362311A (en) * | 2015-11-23 | 2016-03-02 | 安徽科技学院 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
CN106138315A (en) * | 2016-08-09 | 2016-11-23 | 许备占 | Wild lotus lozenge and preparation method thereof |
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EP2223608A4 (en) * | 2007-10-22 | 2010-12-08 | Beijing Dongsheng Agricultural | Abelmoschus manihot (linn.) medius kernel product for natural nutritional edible and pharmaceutical raw material |
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EP2223608A4 (en) * | 2007-10-22 | 2010-12-08 | Beijing Dongsheng Agricultural | Abelmoschus manihot (linn.) medius kernel product for natural nutritional edible and pharmaceutical raw material |
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CN107629874A (en) * | 2017-10-10 | 2018-01-26 | 广东长利香精香料有限公司 | A kind of cinnamomum camphora Verbena officinalis essential oil |
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Effective date of registration: 20170825 Address after: 510000 Guangdong Province, Guangzhou Baiyun District Zhuliao Qing Road, Hongqi Village Industrial Zone No. 38 six Patentee after: Guangzhou creates Cosmetics Co., Ltd. Address before: 233100 east suburb, east suburb of mussel mountain, Bengbu, Anhui 2, unit 13, East 203, China Patentee before: Anhui Science and Technology University |