CN108125929A - It is a kind of12C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules - Google Patents
It is a kind of12C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules Download PDFInfo
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Abstract
The invention discloses one kind12C6+Herba Origani Vulgaris quintessence oil is added in the mixed liquor of chitosan and gutta-percha, while adds in emulsifier by the method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, after being included, is used12C6+Ion beam is irradiated, and obtains Herba Origani Vulgaris quintessence oil microcapsules.This method does not need to initiator, and free from admixture group introduces, products pure；The polymerization of any monomer or the graft modification applied to chitosan and gutta-percha can be used for, this to cause12C6+Ion irradiation polymerization is in essential oil microcapsules in application, better than many pure chemistry polymerizations；Reaction temperature is wide, almost without pressure requirements, is not limited by system status；Reaction process can be easy to industrialization promotion by the way that conventional chemical industry technical parameter and radiation dose rate is controlled to carry out adjusting control in technique, and have both energy-saving and emission-reduction, environmental protection social effect；Microcapsules technology is applied to essential oil production in prevention Eimeria species application, greatly improving the quality of essential oil product.
Description
Technical field
The present invention relates to one kind12C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules.
Background technology
Wild marjoram (Origanum vuLgare L.) stop dysentery grass is a kind of herbaceous plant of Labiatae Origanum, belongs in tradition
Herbal medicine, northwest is distributed mainly in China, on the south North China to the Changjiang river various regions, belongs to medicinal and edible plant.By including vapor
The extraction to Herba Origani Vulgaris quintessence oil can be achieved in distillation and extraction method, supercritical fluid extraction etc..Herba Origani Vulgaris quintessence oil is faint yellow clear oil
Liquid, containing more than 30 kinds of volatile ingredients, therefore volatility is very strong, it is not easy to preserve, primary bioactive components are Sheep's-parsley
Phenol and Thymol.It not only has antibacterial action, but also the activity with anti-malarial protozoon and coccidia, to murder by poisoning, tender, change
Position, heap-type and Bu Shi eimeria tenellas are all effective, promise to be very much natural, ideal novel chiral synthon.Microcapsules technology rises
Derived from the 1930s, technique is increasingly mature at present, application range gradually expands, such as medicine, food field.The technology energy
It is enough that drug is embedded, it effectively improves natural drug stability, reduce volatility and irritation.Wild marjoram prepared by routine techniques
Essential oil microcapsules, though with good moisture retention, rheological characteristic and lubricity, clinical practice finds the dosage form in animal groups
Easily spread in knitting, easily degraded by the oxidation material in animal body or enzyme, it is difficult to meet certain special circumstances requirements slow release and
Stability limits the application of Herba Origani Vulgaris quintessence oil microcapsules clinically.
By being suitably crosslinked to Herba Origani Vulgaris quintessence oil microcapsules, enhance Herba Origani Vulgaris quintessence oil Microencapsulated Slow, degradation time
Extend.More cross-linking method is studied at present mainly using high-energy ray irradiation cross-linking reaction, it, can without catalyst or initiator
Purity height and nontoxic cross-linking products are obtained, when gamma-rays directly applies to the crosslinking of Herba Origani Vulgaris quintessence oil microcapsules, since energy is higher,
Herba Origani Vulgaris quintessence oil strand generates a large amount of free radicals and is broken, and irradiation results are often carried out to degradation direction.
Invention content
The purpose of the invention is to overcome drawbacks described above, one kind is provided12C6+Ion beam irradiation prepares the micro- glue of Herba Origani Vulgaris quintessence oil
The method of capsule.
The purpose of the present invention implements by the following technical programs：
It is a kind of12C6+Herba Origani Vulgaris quintessence oil is added in chitosan and Cortex Eucommiae by the method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules
In the mixed liquor of glue, while emulsifier is added in, after being included, used12C6+Ion beam is irradiated, and obtains the micro- glue of Herba Origani Vulgaris quintessence oil
Capsule.
Further, the method specifically comprises the following steps：
(1) it dissolves the chitosan in acetum, obtains chitosan solution；Gutta-percha is dissolved in ethyl alcohol, obtains Cortex Eucommiae
Obtained chitosan solution and Cortex Eucommiae sol solution are mixed, obtain chitosan-gutta-percha mixed liquor by sol solution；
(2) chitosan for obtaining step (1)-gutta-percha mixeding liquid temperature control adds in Herba Origani Vulgaris quintessence oil at 35~60 DEG C,
Emulsifier is added in simultaneously, is stirred evenly, is placed in water-bath and is reacted；
(3) step (2) mixture taking-up obtained by the reaction is cooled to room temperature, carries out high rotating speed stirring and emulsifying, adjust body
The pH value of system is placed in water-bath and is stirred reaction；
(4) step (3) mixture obtained by the reaction is taken out, ice bath to 6~8 DEG C, the pH value of regulation system adds in crosslinking
Agent is placed in water-bath and is stirred curing, then filters, and obtains wet capsule；
(5) the wet capsule for obtaining step (4) is used12C6+Ion beam is irradiated, and is then washed, dried to get wild marjoram
Essential oil microcapsules.
Further, in the step (1), the mass ratio of chitosan and gutta-percha is 1:1.
Further, in the step (2), addition and chitosan and the Cortex Eucommiae in step (1) of the Herba Origani Vulgaris quintessence oil
The volume mass ratio of glue is 0.5:1~8:1；
The emulsifier is the WJE-880 emulsifiers of Shanghai Wanjin Adjuvant Co., Ltd.；
The temperature of the reaction is 35~60 DEG C, and the time is 2.5~4.5h.
As preference, in the step (2), addition and chitosan and the Cortex Eucommiae in step (1) of the Herba Origani Vulgaris quintessence oil
The volume mass ratio of glue is 2:1；
The temperature of the reaction is 45 DEG C, time 3.5h.
Further, in the step (3), the rotating speed of the high rotating speed stirring and emulsifying is 4000~12000r/min,
Mixing time is 2min；
For the pH value of regulation system to 4.0, pH adjusting agent is 1mol/L acetums；
Described be stirred to react carries out 15min with 250r/min.
As preference, in the step (3), the rotating speed of the high rotating speed stirring and emulsifying is 8000r/min.
Further, in the step (4), for the pH value of regulation system to 7.0, pH adjusting agent is that the NaOH of 1mol/L is molten
Liquid；
The crosslinking agent is glutaraldehyde；
The stirring curing carries out 20min with 250r/min.
Further, in the step (5),12C6+The irradiation dose of ion beam is 100~800Gy.
As preference, in the step (5),12C6+The irradiation dose of ion beam is 400Gy.
Herba Origani Vulgaris quintessence oil volatility is stronger, easily loses during storage.Heavy ion is a kind of emerging drug crosslinking source,
Due to its research in terms of drug molecule and biomolecule modification, linear energy transfer (LET) height and unique ionization peak
(Bragg peaks) accurately controls the unique advantages such as incident depth and position.The present invention is by Herba Origani Vulgaris quintessence oil chitosan and gutta-percha
After being included, carry out12C6+Ion irradiation obtains, and is that inventor tests a kind of effective means found for many years, can be effective
Ground prevents the oxidation and loss of Herba Origani Vulgaris quintessence oil, realizes its lasting bioactivity.
The invention has the advantages that：
(1) this method does not need to initiator, and free from admixture group introduces, products pure；
(2) polymerization of any monomer or the graft modification applied to chitosan and gutta-percha can be used for, this to cause12C6+From
Sub- irradiation polymerization method is in essential oil microcapsules in application, better than many pure chemistry polymerizations；
(3) reaction temperature is wide, almost without pressure requirements, is not limited by system status；
(4) reaction process can be by controlling conventional chemical industry technical parameter and radiation dose rate adjusted in technique and control
System, be easy to industrialization promotion, and have both energy-saving and emission-reduction, environmental protection social effect；
(5) microcapsules technology is applied to essential oil production in prevention Eimeria species application, greatly improving essential oil product
Quality.
Description of the drawings
Fig. 1 is the volatile ingredient total ion current figure of Herba Origani Vulgaris quintessence oil microcapsules；
Fig. 2 is Herba Origani Vulgaris quintessence oil (A), chitosan and gutta-percha (B), Herba Origani Vulgaris quintessence oil microcapsules (C), non-irradiated wild marjoram after irradiation
The infrared spectrum of essential oil microcapsules (D)；
Fig. 3 is the infrared spectrogram of gutta-percha.
Specific embodiment
For more prominent the objectives, technical solutions, and advantages of the present invention, with the following Examples, to the present invention into traveling
One step illustrates, but does not therefore limit the present invention within scope of embodiments.
First, the preparation of Herba Origani Vulgaris quintessence oil microcapsules
1 material
Herba Origani Vulgaris quintessence oil analyzes pure magnificent crude vegetal refinery；The pure raw work biology of chitosan analysis；Gutta-percha：Chinese agriculture
The Lanzhou herding of the industry academy of sciences and the medicament chamber preparation of veterinary drug research institute.WJE-880 analyzes pure Shanghai Wanjin Adjuvant Co., Ltd., remaining
Chemical reagent analyzes pure Tianjin chemical reagent work.
2 irradiance methods
Irradiation experiment carries out in Lanzhou heavy ion research device (HIRFL) biological irradiation terminal.Primary power is
270MeV/u's12C6+Ion beam irradiation sample (Herba Origani Vulgaris quintessence oil after the nickel window of beam current tube, ionisation chamber, air and drop energy piece
Microcapsules), injection rate is monitored with air ionization chamber, sample is replaced and data acquisition is controlled by computer, and all processes are in room
It is carried out under mild Atmospheric Condition, irradiation dose is respectively 0,100,200,400,800Gy, dosage rate 50Gy/min.
3 instrument and equipments
MXR serial experiments room high-shear emulsion machine Shanghai Mu Xuan Industrial Co., Ltd.s；NOVEL-300M microscopes Ningbo is forever
New optics limited company；85-2 constant temperature blender with magnetic force Changzhou national power experimental facilities research institute；Digital display electric work blender
Changzhou Guohua Electric Appliance Co., Ltd.；EYEL water-bath Shanghai Ai Lang Instrument Ltds；Electric heating constant-temperature blowing drying box Shanghai one
Permanent Science and Technology Ltd.；RE52-98 Rotary Evaporators Shanghai Yarong Biochemical Instrument Plant；HH-42 fast constant temperature digital display water tanks Changzhou
Guo Hua Electrical Appliances Co., Ltd；SHB-D micro-vacuum pump using circulatory waters Zhengzhou Greatwall Scientific Industrial ＆ Trading Co., Ltd..
The preparation method of 4 gutta-percha
4.1 material
Folium cortex eucommiae is purchased from Longnan of Gansu Province Chinese Medicinal Materials Markets, the preservation of refrigerator freezing layer is put into after drying in the shade, with 50% after crushing
Ethanol as solvent, the ultrasonic extraction 40min under the conditions of 50~60 DEG C, vacuum filtration, filtrate is for chlorogenic acid extracting and flavones etc.
Medicinal ingredient, filter residue spontaneously dry, and Eucommia ulmoides leave dregs are obtained, for extracting gutta-percha.
Petroleum ether (boiling range is 60~90 DEG C) analysis is pure
4.2 instrument and equipment
Buddhist nun's high-tensile strength infrared spectrometer Nicolet iS10 FTIR spectrum analyzers；High speed Universal pulverizer, Tianjin
Stettlen Instrument Ltd. of city；Ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd..
4.3 preparation method
4.3.1 petroleum ether extracts
6g Eucommia ulmoides leave dregs raw materials are weighed, are Extraction solvent with petroleum ether (boiling range is 60~90 DEG C), are 1 according to solid-liquid ratio:
20 (g/ml), are put into three-necked flask, are filtered to remove filter residue while hot after heating stirring reflux extraction 2h, filtrate slightly cools down and is put into
Refrigerator is filtered by vacuum after cooling crystallization 1h under the conditions of -20 DEG C, is spontaneously dried and be can obtain gutta-percha crude extract.
4.3.2 the thick glue product of Cortex Eucommiae is refined
N-hexane is added in gutta-percha crude extract, volume mass is than 1:20 (g/ml), are stirred at reflux at 40 DEG C
0.5h, it is dry after filtering, obtain canescence essence glue.
4.3.3 the infrared spectrum measurement of gutta-percha
The infrared spectrum of smart glue is measured with liquid-film method：In a heated condition, refined gutta-percha product is dissolved in right amount
Petroleum ether in, Cortex Eucommiae sol solution is made, is uniformly applied in KBr tablettings, it is infrared with Fourier after petroleum ether volatilization completely
Spectrometer measures the infrared spectrum of gutta-percha, sees Fig. 3.
4.4 conclusion
4.4.1 the infrared spectrogram of Fig. 3 gutta-percha and standard items collection of illustrative plates are completely the same.
4.4.2 gutta-percha is extracted in aforementioned manners, and method is simple and practicable, without using water, does not generate waste liquid, solvent is recyclable
It utilizes, the extraction process time is short, and effective comprehensive utilization exploitation for folium cortex eucommiae provides reliable experimental basis.
The preparation of 5 Herba Origani Vulgaris quintessence oil microcapsules
5.1 preparation method
1.00g chitosans are weighed to be dissolved in the acetum of a concentration of 1wt% of 100mL, it is spare；Weigh 1.00g Cortex Eucommiaes
Glue, with 100mL volumetric flask constant volumes after the dissolving of 10mL ethyl alcohol, after two liquid are poured into the beaker of 500mL, be uniformly mixed, mixing
When the temperature of liquid controls 35~60 DEG C, Herba Origani Vulgaris quintessence oil is added in, while add in 300 μ L emulsifier WJE-880, stirred evenly, sealed
It is placed in water-bath and is reacted.After inclusion, taking-up is cooled to room temperature, with high rotating speed stirring and emulsifying 2min, with the vinegar of 1mol/L
The pH of acid solution regulation system is 4.0, is placed in 50 DEG C of water-bath and stirs 15min with the rotating speed of 250r/min, is taken out, ice bath
To 6~8 DEG C, the pH with the NaOH solution regulation system of 1mol/L is 7.0, adds in 200 μ L glutaraldehyde solutions, is placed in 50 DEG C of water
Curing 20min is stirred with the rotating speed of 250r/min in bath, filters to obtain wet capsule product, the wet capsule product of gained is placed on heavy ion research
On the turntable of device biological irradiation, use12C6+Ion beam is irradiated, and the product after irradiation is washed three times with absolute ethyl alcohol, 45
It DEG C is dried in vacuo up to the Herba Origani Vulgaris quintessence oil microcapsule product after being crosslinked.
5.2 process optimization
5.2.1 best core wall ratio is determining
When fixed reaction temperature controls 45 DEG C, irradiation dose 400Gy, reaction time 3.5h, emulsification rotating speed 8000r/min.
It investigates core wall body and accumulates mass ratio to influence of the Herba Origani Vulgaris quintessence oil microcapsules to yield, the results are shown in Table 1.
1 core wall body of table accumulates influence of the mass ratio to yield
| Number | Herba Origani Vulgaris quintessence oil/(chitosan+gutta-percha 1:1)mL/g | Yield % |
| 1 | 0.5:1 | 50.8 |
| 2 | 1:1 | 55.2 |
| 3 | 2:1 | 61.9 |
| 4 | 4:1 | 61.2 |
| 5 | 8:1 | 61.0 |
As shown in Table 1, with Herba Origani Vulgaris quintessence oil/(chitosan+gutta-percha 1:1) raising of the volume mass than mL/g, product are received
Rate increases significantly, but when Herba Origani Vulgaris quintessence oil/(chitosan+gutta-percha 1:1) volume mass ratio is increased to 2:After 1, yield increase is not
Significantly, and wastage of material is caused.Therefore, Herba Origani Vulgaris quintessence oil/(chitosan+gutta-percha 1:1) volume mass ratio can be controlled in 0.5:1
~8:1, best volume mass ratio is 2:1.
5.2.2 best irradiation dose is determining
Fixed core wall body product mass ratio is 2:1, when reaction temperature controls 45 DEG C, reaction time 3.5h emulsifies rotating speed
8000r/min.Irradiation dose is investigated to influence of the Herba Origani Vulgaris quintessence oil microcapsules to yield, the results are shown in Table 2.
Influence of 2 irradiation dose of table to yield
| Number | Irradiation dose/Gy | Yield % |
| 1 | 0 | 61.11 |
| 2 | 100 | 63.77 |
| 3 | 200 | 64.44 |
| 4 | 400 | 67.25 |
| 5 | 800 | 64.16 |
As shown in Table 2, with the raising of irradiation dose, product yield increases significantly, but after irradiation dose 400Gy, receives
Rate does not increase, and illustrating that dosage is big to raw material has destruction.Therefore, 100~800Gy, best irradiation dose are can be controlled in
For 400Gy.
5.2.3 optimal reaction temperature determines
Fixed core wall body product mass ratio is 2:1, irradiation dose 400Gy, reaction time 3.5h, emulsification rotating speed 8000r/min.
Influence of the reaction temperature to yield is investigated, the results are shown in Table 3.
Influence of 3 reaction temperature of table to yield
| Number | Reaction temperature/DEG C | Yield % |
| 1 | 35 | 47.5 |
| 2 | 40 | 51.9 |
| 3 | 45 | 59.6 |
| 4 | 50 | 57.9 |
| 5 | 60 | 57.7 |
As shown in Table 3, with the raising of reaction temperature, product yield increases, but when reaction temperature is more than 45 DEG C, yield increases
Adduction unobvious, and cause wastage of material.Therefore, reaction temperature can be controlled in 35~60 DEG C, and best volume mass ratio is
45℃。
5.2.4 optimum reacting time determines
Fixed core wall body product mass ratio is 2:1, irradiation dose 400Gy, reaction temperature control 45 DEG C, emulsification rotating speed 8000r/
min.The influence of reaction time on yield is investigated, the results are shown in Table 4.
The influence of 4 reaction time on yield of table
| Number | Reaction time/h | Yield % |
| 1 | 2.5 | 45.4 |
| 2 | 3.0 | 49.8 |
| 3 | 3.5 | 56.1 |
| 4 | 4.0 | 55.4 |
| 5 | 4.5 | 55.6 |
As shown in Table 4, with the increase in reaction time, product yield increases, but when reacted between be more than 3.5h, yield increasing
Adduction unobvious.Therefore, the reaction time can be controlled in 2.5~4.5h, and the best reaction time is 3.5h.
5.2.5 optimum emulsification rotating speed is determining
Fixed core wall body product mass ratio is 2:1, irradiation dose 400Gy, reaction temperature control 45 DEG C, and the reaction time is
3.5h.Influence of the emulsification rotating speed to yield is investigated, the results are shown in Table 5.
Table 5 emulsifies influence of the rotating speed to yield
| Number | Emulsify rotating speed/r/min | Yield % |
| 1 | 4000 | 48.3 |
| 2 | 6000 | 52.6 |
| 3 | 8000 | 59.3 |
| 4 | 10000 | 58.6 |
| 5 | 12000 | 58.4 |
As shown in Table 5, with the increase of emulsification rotating speed, product yield increases, but when reaction emulsification rotating speed is more than 8000r/
Min, yield increase are not obvious.Therefore, reaction emulsification rotating speed can be controlled in 4000~12000r/min, best reaction emulsification
Rotating speed is 8000r/min.
2nd, the anti-chicken coccidiasis activity test of Herba Origani Vulgaris quintessence oil microcapsules
1 material
The white plumage cock of 1 age in days, Gansu Kai Yue chicken farms provide, and are raised under the conditions of non-ball worm to 15 ages in days.Tender Amy
That coccidia (Eimeria tenella) Sporulated Oocysts, parasitic disease research department of Lanzhou Veterinary Inst., Chinese Acedemy of Agaricultural Sciences
It provides.
The preparation of 2 Herba Origani Vulgaris quintessence oil microcapsules
1.00g chitosans are weighed to be dissolved in the acetum of a concentration of 1wt% of 100mL, it is spare；Weigh 1.00g Cortex Eucommiaes
Glue, with 100mL volumetric flask constant volumes after the dissolving of 10mL ethyl alcohol, after two liquid are poured into the beaker of 500mL, be uniformly mixed, mixing
When the temperature of liquid controls 45 DEG C, the volume for adding in Herba Origani Vulgaris quintessence oil is 4mL, then core wall body product mass ratio is followed successively by 2:1, it adds in simultaneously
300 μ L emulsifier WJE-880, stir evenly, and sealing, which is placed in water-bath, reacts 3.5h, controls 45 DEG C of reaction system.After inclusion,
Taking-up is cooled to room temperature, and 2min is emulsified with the rotating speed of 8000r/min, and the pH with the acetum regulation system of 1mol/L is 4.0,
It is placed in 50 DEG C of water-bath and 15min is stirred with the rotating speed of 250r/min, take out, ice bath is to 6~8 DEG C, with the NaOH of 1mol/L
The pH of solution regulation system is 7.0, adds in 200 μ L glutaraldehyde solutions, is placed in 50 DEG C of water-bath and is stirred with the rotating speed of 250r/min
Curing 20min is mixed, filters to obtain wet capsule product.The wet capsule of gained is placed on the turntable of heavy ion research device biological irradiation, with 0,
, 400,100th, 200 800Gy dosage12C6+Ion beam is irradiated, and the product after irradiation is washed three times with absolute ethyl alcohol, 45
It DEG C is dried in vacuo up to the microcapsule product after being crosslinked.
3 analysis determination conditions
Agilent companies of the 6890N-5973i gas chromatograph-mass spectrometers U.S., the 10 high limited public affairs of dove industry and trade in μ L microsyringes Shanghai
Department.
Chromatographic condition：DB-MS capillary columns (30m × 0.25mm, 0.25 μm), carrier gas are helium, flow velocity 1mL/min；Into
260 DEG C of sample mouth temperature, split ratio 30:1；Temperature program：50 DEG C of initial temperature (retains 2min), and 90 DEG C are risen to 8 DEG C/min,
180 DEG C are risen to 4 DEG C/min again, finally rises to 300 DEG C with 10 DEG C/min.
Mass Spectrometry Conditions：EI ionization sources, electron bombardment energy 70eV；230 DEG C of ion source temperature；150 DEG C of quadrupole rod temperature；Matter
Measure 25~450amu of scanning range；280 DEG C of auxiliary temperature；Tune file stune.u；Scan pattern Scan.
Sample treatment:0.5g Herba Origani Vulgaris quintessence oil microcapsules are taken, 10mL ether is added to be heated to reflux in 50mL round-bottomed flasks
30min after crossing filter solid, boils off ether on a rotary evaporator.After the special membrane filtration of gas chromatograph-mass spectrometer sample, use is micro
Sample introduction needle takes 0.6 μ L Herba Origani Vulgaris quintessence oils to be injected separately into the injection port of GC-MS and GC-O, and split ratio is set as 30:1.
The volatile ingredient total ion current figure of Herba Origani Vulgaris quintessence oil microcapsules is shown in Fig. 1.Different irradiation dose Herba Origani Vulgaris quintessence oil microcapsules
Carvacrol, Thymol and yield are shown in Table 6.
The different irradiation dose Herba Origani Vulgaris quintessence oil microcapsules of table 6 prepare result
| Irradiation dose/Gy | Carvacrol % | Thymol % | Yield % |
| 0 | 0.502 | 0.201 | 61.11 |
| 100 | 0.503 | 0.201 | 63.77 |
| 200 | 0.503 | 0.201 | 64.44 |
| 400 | 0.502 | 0.200 | 67.25 |
| 800 | 0.501 | 0.200 | 64.16 |
4 are changed with the front and rear Herba Origani Vulgaris quintessence oil microcapsules of infrared spectroscopic determination crosslinking
Appropriate chitosan and the Herba Origani Vulgaris quintessence oil microcapsules after gutta-percha, predose are taken, is ground, made after tabletting infrared with KBr
Spectral scan, and IR spectrum scanning is carried out to Herba Origani Vulgaris quintessence oil, Infrared spectra adsorption curve is made, sees Fig. 2.
The grouping and processing of 5 experimental animals
70 15 Japanese instar chicklings are randomly divided into 7 groups by weight, including Herba Origani Vulgaris quintessence oil microcapsules (5 after crosslinking
Dosage), infect control group and healthy control group.15 ages in days start to add a certain proportion of said medicine in feed, wild marjoram essence
Oil microcapsule each group additive capacity is according to Ministry of Agriculture addition specified amount 100mg/kg.In addition to healthy control group, remaining each group is equal
The peroral infection Eimeria tenella Sporulated Oocysts 4.0 × 10 in 15 age in days4/ only.Then it raises to 22 ages in days.
6 curative effect of medication deliberated indexes and standard
6.1 test chickens survey weight by total Test chicken respectively at 15 ages in days and 22 ages in days by only surveying weight, and by with
Lower formula calculates body weight increase rate.Body weight increase rate=test group average growth rate/healthy control group average growth rate ×
100%.
6.2 is clinical and pathological observation experiment during situations such as observing the spirit of each group chicken, appetite, excrement, death daily,
And record result.It is autopsied to chicken dead during experiment, observes its Pathologic changes.
When 6.3 chicken caecum lesions check 22 age in days, the test chicken all survived is slaughtered, disease is carried out by caecum and small intestine is only taken
Reason checks, scores by the lesion score method of Johnson and Reid, then calculates pathological changes value by the method for angle Tian Qing.Disease
Variate=every group of average lesion scores × 10.
Caecum lesion standards of grading：Caecum is normally 0 point without egg capsule；There is egg capsule, caecum mucous membrane thickens, and has a small amount of being dispersed in property
Bleeding is 1 point；There is egg capsule, caecum mucous membrane thickens, and it is 2 points to have apparent blood or blood content；There is egg capsule, caecum mucous membrane increases
Thickness, it is 3 points to have a large amount of blood clots or blood sample intestines core；There is egg capsule, caecum appearance is in dark reddish brown, hence it is evident that swelling, content blood sample are 4
Point；Because coccidium infection death also calculates 4 points.
The coccidian oocyst inspection of 6.4 test chickens looks into egg capsule with erythrocyte counting method.The caecum of every group of test chicken is scraped respectively
Content is counted after being sufficiently stirred mixing with conventional method, and calculates the egg sac number (O.P.G) of every gram of excrement, then by angle Tian Qing
Method calculate oocyst value.
The computational methods of oocyst value：The O.P.G values of 7d chickens and the ratio of the O.P.G values of not administration group chicken are less than after infecting
When 1%, oocyst value 0；In 1%-25%, oocyst value 20；In 75%-100%, oocyst value 40.
6.5 effects are judged according to the body weight increase rate of each group test chicken, survival rate, pathological changes value and oocyst value, according to Merck
The calculation formula of company calculates anticoccidial index (ACI)：ACI=(body weight increase rate+survival rate) × 100- (pathological changes values+egg capsule
Value)
Using ACI as its effect of standard determination：ACI ＜ 120 are invalid；ACI=120-160 is inefficient；ACI=160-180
For middle effect；ACI ＞ 180 are efficient.
7 results and discussion
7.1 using chitosan and gutta-percha as wall material, and Herba Origani Vulgaris quintessence oil microcapsules are prepared by heavy ion irradiation, product white,
Uniform little particle.The microcapsule embedded rate of Herba Origani Vulgaris quintessence oil that conventional method preparation is overcome by heavy ion irradiation crosslinking is relatively low,
The problem of embedding rate changes greatly, poor reproducibility.
The infrared spectrum analysis of the infrared spectrum analysis Herba Origani Vulgaris quintessence oil microcapsules of 7.2 Herba Origani Vulgaris quintessence oil microcapsules is as shown in Figure 2.
The circular hollow molecule that chitosan is made of with gutta-percha glucose molecule, if it, which is successfully crosslinked Herba Origani Vulgaris quintessence oil, forms embedding
Object can only be that O-H keys are had an effect.3670-3230cm-1For the stretching vibration absworption peak of O-H keys, 1420-1260cm-1For O-H
The bending vibration absorption peak of key.In chitosan and gutta-percha (spectrogram B), the feature stretching vibration absworption peak of O-H keys is 3388cm-1, and after irradiation in Herba Origani Vulgaris quintessence oil microcapsules (spectrogram C), this characteristic peak increases 3394cm-1；In addition, chitosan with
In gutta-percha (spectrogram B), the characteristic flexural vibration absorption peak of O-H keys is 1411cm-1, and Herba Origani Vulgaris quintessence oil microcapsules (spectrum after irradiating
Figure C) in corresponding characteristic peak increase 1417cm-1.The combination of hydroxyl and hydrogen bond results in vibration frequency decline, infrared absorption
Peak is moved to long wave, and hydroxyl and Hydrogenbond intensity are bigger, and long wave movement is more serious.The Herba Origani Vulgaris quintessence oil for not carrying out cross-linking radiation is micro-
Capsule (spectrogram D) is clearly distinguishable from crosslinked spectrogram.It can be seen that Herba Origani Vulgaris quintessence oil is crosslinked successfully i.e. by chitosan with gutta-percha
Through crosslinked chitosan and gutta-percha/Herba Origani Vulgaris quintessence oil microcapsules are successfully made.
3d after 7.3 clinical test of pesticide effectiveness inoculation coccidias, other test group chickens show different journeys in addition to healthy control group
The clinical symptoms of degree, such as feed intake is reduced, feather is fluffy and disorderly, both wings are sagging, drop-head necking down, eye closing lethargic sleep, be reluctant to walk about, peel off it is slow-witted
Vertical, discharge bloody stool etc..4-5d after inoculation coccidia, infection control group chicken row go out a large amount of bloody stool, the blood of all administration group test chickens
Just it significantly reduces, mental status and feed intake are clearly better, and each group chicken does not occur death during entire experiment.
7.4 pathological anatomy variation test chicken is all slaughtered in 22 ages in days, and pathological anatomy is found, healthy control group chicken owns
Internal organs are normal；Control group chicken caecum and the notable swelling of duodenum are infected, includes a large amount of blood sample contents；All administration group examinations
Chicken caecum and duodenum are tested although also there is swelling, blood sample content, lesion degree is substantially reduced, other are dirty for test chicken
Device has no that apparent eye sees lesion.
Clinical symptoms and the pathological anatomy variation of the anticoccidial effect compbined test chicken of 7.5 Herba Origani Vulgaris quintessence oil microcapsules, lead to
It crosses the indexs such as body weight increase rate, survival rate, oocyst value and pathological changes value and calculates ACI, the results show that passing through wild marjoram after Ion Irradiation on Multi-walled Carbon
The ACI of essential oil microcapsules in 160-180, has medium anticoccidial effect, and the ACI of non-irradiated essential oil microcapsules is
151.81, belong to low anticoccidial effect.Illustrate after being crosslinked by heavy ion irradiation, in vivo with certain slow releasing function, anticoccidial
Index improve, but irradiation dose be more than 400Gy when, the chemical composition of essential oil may be destroyed.It the results are shown in Table 7.
The anticoccidial effect of 7 Herba Origani Vulgaris quintessence oil microcapsules of table
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although with reference to aforementioned reality
Example is applied the present invention is described in detail, it for those skilled in the art, still can be to aforementioned each implementation
Technical solution recorded in example modifies or carries out equivalent replacement to which part technical characteristic.All essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
- It is 1. a kind of12C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that gather Herba Origani Vulgaris quintessence oil addition shell In the mixed liquor of sugar and gutta-percha, while emulsifier is added in, after being included, used12C6+Ion beam is irradiated, and obtains wild marjoram Essential oil microcapsules.
- It is 2. according to claim 112C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute The method of stating specifically comprises the following steps：(1) it dissolves the chitosan in acetum, obtains chitosan solution；Gutta-percha is dissolved in ethyl alcohol, obtains Cortex Eucommiae peptization Obtained chitosan solution and Cortex Eucommiae sol solution are mixed, obtain chitosan-gutta-percha mixed liquor by liquid；(2) chitosan for obtaining step (1)-gutta-percha mixeding liquid temperature control adds in Herba Origani Vulgaris quintessence oil, simultaneously at 35~60 DEG C Emulsifier is added in, is stirred evenly, is placed in water-bath and is reacted；(3) step (2) mixture taking-up obtained by the reaction is cooled to room temperature, carries out high rotating speed stirring and emulsifying, regulation system PH value is placed in water-bath and is stirred reaction；(4) step (3) mixture obtained by the reaction being taken out, ice bath to 6~8 DEG C, the pH value of regulation system adds in crosslinking agent, It is placed in water-bath and is stirred curing, then filter, obtain wet capsule；(5) the wet capsule for obtaining step (4) is used12C6+Ion beam is irradiated, and is then washed, dried to get Herba Origani Vulgaris quintessence oil Microcapsules.
- It is 3. according to claim 212C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (1), the mass ratio of chitosan and gutta-percha is 1:1.
- It is 4. according to claim 212C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (2), addition and the volume mass of the chitosan and gutta-percha ratio in step (1) of the Herba Origani Vulgaris quintessence oil are 0.5:1 ~8:1；The emulsifier is the WJE-880 emulsifiers of Shanghai Wanjin Adjuvant Co., Ltd.；The temperature of the reaction is 35~60 DEG C, and the time is 2.5~4.5h.
- It is 5. according to claim 412C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (2), addition and the volume mass of the chitosan and gutta-percha ratio in step (1) of the Herba Origani Vulgaris quintessence oil are 2:1；The temperature of the reaction is 45 DEG C, time 3.5h.
- It is 6. according to claim 212C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (3), the rotating speed of the high rotating speed stirring and emulsifying is 4000~12000r/min, mixing time 2min；For the pH value of regulation system to 4.0, pH adjusting agent is 1mol/L acetums；Described be stirred to react carries out 15min with 250r/min.
- It is 7. according to claim 612C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (3), the rotating speed of the high rotating speed stirring and emulsifying is 8000r/min.
- It is 8. according to claim 212C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (4), for the pH value of regulation system to 7.0, pH adjusting agent is the NaOH solution of 1mol/L；The crosslinking agent is glutaraldehyde；The stirring curing carries out 20min with 250r/min.
- It is 9. according to claim 212C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (5),12C6+The irradiation dose of ion beam is 100~800Gy.
- It is 10. according to claim 912C6+The method that ion beam irradiation prepares Herba Origani Vulgaris quintessence oil microcapsules, which is characterized in that institute It states in step (5),12C6+The irradiation dose of ion beam is 400Gy.
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