A kind of preparation method of zedoary volatile oil clathrate
Technical field
The present invention relates to the inclusion processing technique fields of Chinese medicine effective ingredient volatile extract, specifically a kind of
The preparation method of zedoary volatile oil clathrate.
Background technology
Contain volatile oil in several kinds of Chinese medicinal materials, but volatile oil itself is unstable, it is added without processing, Direct spraying
Its active ingredient is readily volatilized in product made of particle method, aoxidizes, and the loss amount of volatile oil is larger, and manufactured product can be direct
The effect of influencing pharmaceutically-active performance, leading to drug declines;Due to differing for storage requirement, different batches production is also resulted in
Quality is inhomogenous.It is using β-ring paste to increase stability of volatile oil at present and cover the common method of volatile oil penetrating odor
Smart (β-cyclodextrin, β-CD) is included, and makes liquid medicine powdered, convenient for a variety of different dosage forms are made.Volatilization
Oil can reduce the volatilization of volatile ingredient after inclusion, reduce the irritation of drug, the disadvantage for overcoming dosage not easy to control, effectively
The stability for improving product quality, to improve the stability and curative effect of drug.
Oil of zedoary turmeric is the volatile oil extracted through steam distillation in Traditional Chinese medicine Rhizoma curcumae, has antitumor, antibacterial, disease-resistant
The multiple pharmacological effects such as poison, antithrombotic, liver protection, anti-psoriasis and enhancing immune function.A variety of aromatic turmeric oil preparations are successful
Applied to clinic.Oil of zedoary turmeric has the shortcomings of not soluble in water, poor bioavailability, bitter, is directly added into particle and is made
Solid pharmaceutical preparation such as capsule, granule when, volatile oil highly volatile and Odor stimulation are big, are not easy to take orally, this is just limited
The application of oil of zedoary turmeric.And smelly flavoring can be rectified by forming inclusion compound with cyclodextrin, prevented the volatilization of oil of zedoary turmeric, enhanced oil of zedoary turmeric
Stability increases its water solubility, improves its bioavilability.
The method of inclusion essential oil mainly has polishing, saturated water solution method, ultrasonic method etc., the volatilization of saturated water solution method
Oily inclusion degree and utilization rate are relatively high, are better than other two methods, therefore generally use saturated water solution method in actual production.
The production method of oil of zedoary turmeric inclusion complex has saturated water solution method, also there is polishing, can form stable inclusion compound.
Saturated water solution method is after preferably:β-CD:Oil (g:Ml it is) 8:1, inclusion temperature be 40 DEG C, the inclusion time for 90min~
120min, refrigeration 20 hours or more filter and obtain inclusion compound, and it is shady and cool dry to place ventilation, obtains oil of zedoary turmeric inclusion compound.It presses《China
People's republic's pharmacopeia》One Ⅹ D determination of volatile oil methods of annex detection, inclusion essential oil rate are 90.90%, volatile oil utilization rate
It is 66.67%.Hebei Yi Ling Pharmaceutical Groups prepare the oil of zedoary turmeric supported in positive capsule using polishing, by β-CD:Oil of zedoary turmeric (g:
m1): 8:1, add 5 times of water, continuously grinding 100min obtains inclusion compound, filters to dry, then with a small amount of petroleum ether, 50 DEG C
~55 DEG C are dried in vacuo 4 hours, obtain volatile oil clathrate compound.Inclusion rate is between 62.2%~63.7%, average inclusion rate 62.9%.
Invention content:
That the object of the present invention is to provide a kind of volatile oil utilization rates is high, inclusion rate is high and includes time short Curcuma Aromatic Oil
The preparation method of inclusion compound.
A kind of preparation method of zedoary volatile oil clathrate of the present invention, setting inclusion control condition are:Oil of zedoary turmeric and β-ring
Dextrin(Weight/volume)The ratio between be 1: 6,40 DEG C~50 DEG C of temperature of inclusion, the min of inclusion time 30min~45, detailed process and
Steps are as follows:
(1)The purified water a of 10 times of oil of zedoary turmeric (volume) amount is weighed, it is spare;
(2)It takes oil of zedoary turmeric, the ethyl alcohol dissolving of 1/5 times of amount of curcuma zedoary oil volume is added, obtain oil of zedoary turmeric ethyl alcohol lysate b, it is spare;
(3)It with reference to colloid mill specification, is first carried out disinfection to colloid mill with appropriate 75% ethyl alcohol, controls colloid mill rotating speed
1500~3500rpm, then b is passed through in colloid mill, the slurries in colloid mill are rinsed with a, until the water outlet for rinsing colloid mill is in nothing
Color, it is c that this oil of zedoary turmeric ethyl alcohol lysate for crossing colloid mill acquisition, which is in emulsion form,;
(4)The beta-cyclodextrins (g/ml) for taking 6 times of oil of zedoary turmeric amount, add remaining purified water in a, after heating for dissolving, are cooled to
40 DEG C~50 DEG C, obtain the saturated aqueous solution d of beta-cyclodextrin;
(5)C is added slowly in d, stirring while adding, mixing speed is 1000~2000rpm, continues to stir after adding
The min of 30min~45, then be placed in 0 DEG C~4 DEG C environment and refrigerate, stand 12 hours;
(6)Then it filters to dry, then precipitation is washed with a small amount of ethyl alcohol, filtrate discards, and obtains volatile oil clathrate compound;
(7)Volatile oil inclusion complex is dried at 50 ± 5 DEG C, is ground into fine powder,.
Zedoary volatile oil clathrate made from the above method is pressed《Pharmacopoeia of People's Republic of China》2010 editions annex Ⅹ
D determination of volatile oil methods detect, and for volatile oil oil utilization rate up to 85% or more, inclusion rate is 95% or more.
It tests and investigates through influence factor, the oil of zedoary turmeric inclusion compound of the oil of zedoary turmeric preparation method acquisition of patent of the present invention does not have
It degrades.
The preparation method of the zedoary volatile oil clathrate of the present invention, setting control condition are:Oil of zedoary turmeric and beta-cyclodextrin body
The ratio between product is 1: 6,40 DEG C~50 DEG C of temperature of inclusion, the min of inclusion time 30min~45, first using passing through colloid in operating procedure
The preparation method that mill is emulsified, again included emulsion and β-CD with saturated water solution method, inclusion time are obviously shortened, and volatilize
The utilization rate and inclusion rate of oil significantly improve, and have the advantages that production efficiency height, product quality are stablized, and are suitble to extensive raw
Production.
Specific implementation mode
Below by following embodiment, the invention will be further described, it will be helpful to understand the present invention, but and unlimited
Present disclosure processed.
Embodiment 1
With a kind of preparation method of zedoary volatile oil clathrate of the present invention, for the 2kg/ that feeds intake batches of Curcuma Aromatic Oils,
Operating process and steps are as follows:
(1)The purified water a of the i.e. 20L of 10 times of curcuma zedoary oil volume amount is weighed, it is spare;
(2)Oil of zedoary turmeric is taken, the ethyl alcohol dissolving that 1/5 times of amount of curcuma zedoary oil volume is 0.4L is added, obtains oil of zedoary turmeric ethyl alcohol lysate
B, it is spare;
(3)It with reference to colloid mill specification, is first carried out disinfection to colloid mill with appropriate 75% ethyl alcohol, controls colloid mill rotating speed
1500rpm, then by b, that is, oil of zedoary turmeric ethyl alcohol lysate input colloid mill, the slurries in colloid mill are rinsed with 2L-3L a, until punching
The water outlet for washing colloid mill is in colourless, and it is c that this oil of zedoary turmeric ethyl alcohol lysate for crossing colloid mill acquisition, which is in emulsion form,;
(4)Take the beta-cyclodextrin (g of 6 times of i.e. 12L of amount of oil of zedoary turmeric:Ml), remaining purified water a is added, mixes, is heated to 55
DEG C dissolving after, be cooled to 50 DEG C, obtain the saturated aqueous solution d of beta-cyclodextrin;
(5)It was that the oil of zedoary turmeric ethyl alcohol lysate that colloid mill obtains is added slowly in d by c, stirring while adding, mixing speed
For 1000rpm, continue to stir 36 min after adding, then is placed in 0 DEG C~4 DEG C environment and refrigerates, stands 12 hours;
(6)Then it filters to dry, then precipitation is washed with a small amount of ethyl alcohol, filtrate discards, and obtains volatile oil clathrate compound;
(7)Volatile oil inclusion complex is dried at 50 ± 5 DEG C, is ground into fine powder, crosses 80 mesh sieve,.
The method that colloid mill emulsification-saturated water solution method in the present embodiment is combined prepares obtained oil of zedoary turmeric inclusion
Object is pressed《Pharmacopoeia of People's Republic of China》2010 editions Ⅹ D determination of volatile oil methods of annex detections, volatile oil oil utilization rate are
88.9%, inclusion rate 97.0%.And examined through thin-layer chromatography, it was demonstrated that oil of zedoary turmeric principal component after inclusion is basically unchanged, through oxygen
The factors influencings such as change, illumination thermal stability, inclusion compound property are stablized, and are verified through technique reproducibility, and reproducibility is good.
Embodiment 2
With a kind of preparation method of zedoary volatile oil clathrate of the present invention, for the 3kg/ that feeds intake batches of Curcuma Aromatic Oils,
Operating process and steps are as follows:
(1)The purified water a of the i.e. 30L of 10 times of curcuma zedoary oil volume amount is weighed, it is spare;
(2)Oil of zedoary turmeric is taken, the ethyl alcohol dissolving that 1/5 times of amount of curcuma zedoary oil volume is 0.6L is added, obtains oil of zedoary turmeric ethyl alcohol lysate
B, it is spare;
(3)It with reference to colloid mill specification, is first carried out disinfection to colloid mill with appropriate 75% ethyl alcohol, controls colloid mill rotating speed
2900rpm, then by b, that is, oil of zedoary turmeric ethyl alcohol lysate input colloid mill, the slurries in colloid mill are rinsed with 2L-3L a, until punching
The water outlet for washing colloid mill is in colourless, and it is c that this oil of zedoary turmeric ethyl alcohol lysate for crossing colloid mill acquisition, which is in emulsion form,;
(4)Take the beta-cyclodextrin (g of 6 times of i.e. 18L of amount of oil of zedoary turmeric:Ml), remaining purified water a is added, mixes, is heated to 45
DEG C dissolving after, be cooled to 40 DEG C, obtain the saturated aqueous solution d of beta-cyclodextrin;
(5)It was that the oil of zedoary turmeric ethyl alcohol lysate that colloid mill obtains is added slowly in d by c, stirring while adding, mixing speed
For 1500rpm, continue to stir 30 min after adding, then is placed in 2 DEG C~4 DEG C environment and refrigerates, stands 12 hours;
(6)Then it filters to dry, then precipitation is washed with a small amount of ethyl alcohol, filtrate discards, and obtains volatile oil clathrate compound;
(7)Volatile oil inclusion complex is dried at 50 ± 5 DEG C, is ground into fine powder, crosses 80 mesh sieve,.
The method that colloid mill emulsification-saturated water solution method in this implementation is combined prepares oil of zedoary turmeric inclusion compound, presses《China
People's republic's pharmacopeia》2010 editions Ⅹ D determination of volatile oil methods of annex detections, volatile oil oil utilization rate are 85.3%, inclusion
Rate is 95.2%.And examined through thin-layer chromatography, it was demonstrated that oil of zedoary turmeric principal component after inclusion is basically unchanged, and oxidized, illumination is hot steady
The factors influencings such as qualitative, inclusion compound property are stablized, and are verified through technique reproducibility, and reproducibility is good.
Embodiment 3
With a kind of preparation method of zedoary volatile oil clathrate of the present invention, for the 1kg/ that feeds intake batches of Curcuma Aromatic Oils,
Operating process and steps are as follows:
(1)The purified water a of the i.e. 10L of 10 times of curcuma zedoary oil volume amount is weighed, it is spare;
(2)Oil of zedoary turmeric is taken, the ethyl alcohol dissolving that 1/5 times of amount of curcuma zedoary oil volume is 0.2L is added, obtains oil of zedoary turmeric ethyl alcohol lysate
B, it is spare;
(3)It with reference to colloid mill specification, is first carried out disinfection to colloid mill with appropriate 75% ethyl alcohol, controls colloid mill rotating speed
3500rpm, then by b, that is, oil of zedoary turmeric ethyl alcohol lysate input colloid mill, the slurries in colloid mill are rinsed with 1L-1.5L a, until
The water outlet for rinsing colloid mill is in colourless, and it is c that this oil of zedoary turmeric ethyl alcohol lysate for crossing colloid mill acquisition, which is in emulsion form,;
(4)Take the beta-cyclodextrin (g of 6 times of i.e. 6L of amount of oil of zedoary turmeric:Ml), remaining purified water a is added, mixes, is heated to 50
DEG C dissolving after, be cooled to 45 DEG C, obtain the saturated aqueous solution d of beta-cyclodextrin;
(5)The saturated aqueous solution liquid for the β-CD that the oil of zedoary turmeric ethyl alcohol that c was colloid mill acquisition dissolves 45 DEG C is added slowly to d
(The saturated aqueous solution of i.e. 45 DEG C of β-CD)In, stirring while adding, mixing speed 2000rpm continues stirring 45 after adding
Min, then be placed in 1 DEG C~3 DEG C environment and refrigerate, stand 12 hours;
(6)Then it filters to dry, then precipitation is washed with a small amount of ethyl alcohol, filtrate discards, and obtains volatile oil clathrate compound;
(7)Volatile oil inclusion complex is dried at 50 ± 5 DEG C, is ground into fine powder, crosses 80 mesh sieve,.
The Curcuma Aromatic Oil inclusion that the method that colloid mill emulsification-saturated water solution method in this implementation is combined prepares
Object is pressed《Pharmacopoeia of People's Republic of China》2010 editions Ⅹ D determination of volatile oil methods of annex detections, volatile oil oil utilization rate are
92.9%, inclusion rate 98.0%.And examined through thin-layer chromatography, it was demonstrated that oil of zedoary turmeric principal component after inclusion is basically unchanged, through oxygen
The factors influencings such as change, light illumination thermal stability, inclusion compound property are stablized, and are verified through technique reproducibility, and reproducibility is good.