A kind of preparation method of five-leaved chaste tree volatile oil
Technical field
The present invention relates to five-leaved chaste tree volatile oil field, is a kind of preparation method of five-leaved chaste tree volatile oil.
Background technology
In foodstuffs industry, sanitas is one of most important additive.It is that a class be take the foodstuff additive that protection food value and original character is object.At present conventional sanitas is in the majority with chemosynthesis sanitas in the world, but luring of chemosynthesis sanitas is carcinous, teratogenecity and the problems such as food chronic poisoning that easily cause have caused social extensive concern.In recent years, along with the raising of people’s life and the level of consumption, the demand of food-processing also more and more changes to directions such as ” greens ” and ” natural “.Therefore, the research and development of natural safe functional foodstuff sanitas just seem more and more important.Antiseptics for natural food can be divided into microbialpreservatives (N,O-Diacetylmuramidase, nisin, tennecetin, epsilon-polylysine), creatural preservative (protamine, propolis, chitosan) and plant source antiseptic agent (tea-polyphenol, plants essential oil, garlicin, anthraquinone herbal medicine).Plants essential oil is wherein a class natural vegetal feed additives, can correct food peculiar smell, give fragrance, painted, anti-oxidant, antibiotic (anticorrosion) and the physiological and pharmacological effect in addition that have.As one of important sources of natural antiseptic agent, from plants essential oil, filter out efficient, economic, safe preservative substance as food preservatives, have broad application prospects and Research Significance greatly.
At present, antibacterial research to plant is a lot, according to its research effect, roughly can be divided into following three kinds: to causing that restraining effect research of the pathogenic bacteria of food spoilage finds natural food preservatives, restraining effect research of phytopathogen is developed modern and restraining effect research of human body pathogenic bacteria is produced to newtype drug.Meanwhile, according to being divided into again the site of action of plant research: extract plants essential oil and carry out antibacterial research, roots of plants, stem, leaf are carried out to antibacterial experiment and the anti-microbial activity research to plant endogenesis fungus extract with organic solvent extraction.
On the basis that the present invention is intended to five-leaved chaste tree volatile oil to extract; be applied to lotus rhizome anti-corrosive fresh-keeping; biocidal property, security as plant-sourced food preservatives; to obtaining green, safe and reliable plant-sourced food preservatives; for the comprehensive development and utilization of five-leaved chaste tree provides experiment basis; improve the utilization ratio of plant resources, create high economic worth.
Five-leaved chaste tree (Vitex negundo Linn) is Verbenaceae Vitex species, another name five-leaved chaste tree bar, Fructus Viticis Negundo, cloth chaste tree, the twigs of the chaste tree, the five fingers wind, Folium vilicis Negundo.It is annual machaka or dungarunga, and plant height can reach 6m, and branch, leaf and stem all have fragrance, from base portion branch, and close raw canescence fine hair.Leaf is to life, and palmately compound leaf, has long handle, leaflet 3-5 sheet, and light green, is ellipticity avette to lanceolar, full edge or slightly sawtooth, the white fine hair of the close life in the back side, rubbing has peat-reek.The suitable existence of five-leaved chaste tree in the torrid zone and Temperate Region in China, is distributed widely in China Yangtze valley and each provinces and regions, south, and also there is distribution in Shandong.Eastern Africa also extensively distributes through the ground such as Bolivia of Madagascar, the southeast, Asia and South America.
Yellow vitex seed, leaf, branch and root all can be used as medicine.Yellow vitex seed has cough-relieving apophlegmatic and alleviates the effect of bronchospasm, cures mainly flu, cough, asthma, wandering arthritis, malaria, stomachache, hernia, anal fistula etc.Negundo Chastetree Leaf can relieving superficies by cooling, eliminating damp, detoxifying, cures mainly flu, heatstroke, vomiting and diarrhoea, dysentery, malaria, jaundice, rheumatism, treating swelling and pain by traumatic injury, sore pain mange, and can prevent the development of formaldehyde sacroiliitis swelling.The decoction of Negundo Chastetree Leaf or root has restraining effect to bacillus such as streptococcus aureus, beta hemolytic streptococcus and large intestine, anthrax, diphtheria, typhoid fever, green pus, dysentery.
Five-leaved chaste tree plants essential oil, also claims perfume oil or volatile oil, is a class plant-sourced secondary metabolism class material, is molecular weight in plant materials, can steams with water vapour, have the volatility oily liquid substance of certain smell.Essential oil is generally to extract fruit, flower, leaf and the root from plant, has strong fragrance or smell.The chemical composition more complicated that it is contained, can be divided into aliphatics, aromatic series and terpene three major types and their containing oxygen derivative as alcohol, aldehyde, ketone, acid, ether, ester, lactone etc. by chemical structure, also has in addition nitrogenous and compound sulfur-bearing.Conventionally plants essential oil is used for preparing essence and flavoring agent, but in the last few years, the anti-microbial activity of plants essential oil and single component thereof has been carried out to a large amount of research both at home and abroad.Research shows, that plants essential oil has is antibacterial, desinsection, anti-oxidant isoreactivity, at aspects such as medicine, agricultural chemicals, fodder additivess, has widespread use.
Five-leaved chaste tree volatile oil has significant comprehensive insecticidal activity to Main Stored Grain Insects such as sitophilus zea-mais, Callosobruchus chinensis, lesser grain borers, and can effectively control Fl for the formation of population, reduces its quantity.Monomer Terpane, firpene all have higher insecticidal activity to corundum Sitophilusspp. imago, are insecticide active substances important in five-leaved chaste tree volatile oil.The employing steam distillations such as Yang Haixia extract volatile oil from five-leaved chaste tree.Utilize gas chromatography/mass spectrometry technology (GC.MS) to study the chemical composition of five-leaved chaste tree volatile oil.Be separated to altogether 37 compounds, identified wherein 28.Mainly comprise caryophyllene (23.981%).Huang Qiong (2008) etc. extract the volatile oil of Vitex negundo var cannabifolia with microwave irradiation, use capillary gas chromatography one MS in conjunction with computer search, its chemical composition is carried out respectively to analysis and identification, by area normalization method, measure the relative content of each compound in volatile oil.Result identifies 16 compounds altogether, and volatilization main body of oil is caryophyllene (20.14%).
Extract the more conventional extracting method of plant volatile oil and have steam distillation (water distillation method, distilling above water method, steam distillation), water diffusion process, solvent extraction method, absorption method, supercritical CO 2abstraction technique, ultrasonic wave auxiliary extraction technology, microwave radiation induction abstraction technique, enzyme extraction technology etc.Shortcoming is to destroy large to heat-sensitive substance and unstable constituents.
Summary of the invention
The object of the invention is to provide a kind of employing simultaneous distillation method, use the preparation method of opposed polarity organic solvent extraction five-leaved chaste tree volatile oil.
Technical scheme of the present invention is, it is characterized in that adopting and weigh 10g five-leaved chaste tree powder in the round-bottomed flask of 1000mL, add 300mL distilled water and make abundant submergence material, separately get 50mL normal hexane in 500mL flask, connect distilling and extracting device simultaneously, make material one end keep about 110 ± 5 ℃ of slight boiling condition temperature, organic solvent-normal hexane one end temperature is controlled at 80 ℃ ± 5 ℃, treating all to reflux in both sides starts timing and maintains 4h, after extraction, organic reagent is transferred in tool plug triangular flask, add anhydrous sodium sulphate to being fine-grannular without large caking, refrigerator overnight, after crossing the millipore filtration of 0.45 μ m, rotary evaporation is to residual on a small quantity, transfer in sample injection bottle and nitrogen blowing to solvent-free smell, obtain yellow volatile oil, there is strong peat-reek, this essential oil is carried out to GC-MS on-line analysis, organic reagent normal hexane is changed and makees hexanaphthene (90 ℃ ± 5 ℃ of temperature), methylene dichloride (50 ℃ ± 5 ℃), ethyl acetate (90 ℃ ± 5 ℃) and use the same method and carry out while distillation extraction, distillation extraction is that sample aqueous solution and organic reagent are placed in respectively to the both sides of instrument and are heated to boiling simultaneously, water vapor and solvent vapo(u)r fully mix in device, simultaneously condensation is got off and the organic solvent component in aqueous phase extracted constantly still in the process dirty along prolong, because water and organic phase are not dissolved each other in U-shaped pipe and to be separated, be back to respectively in the flask of both sides, through distillation, extraction process continuous, circulation, reach the object of the volatile and semi-volatile compounds of trace in extraction, separation and enrichment sample.
Owing to having adopted technique scheme, the extractive technique of screening has extraction yield feature high, simple to operate; Be used for the fresh-keeping of fresh lotus rhizome, effect is excellent; Contribute to improve the content of target compound.