CN104027387B - A kind of preparation method of dalbergia wood distillate - Google Patents
A kind of preparation method of dalbergia wood distillate Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of dalbergia wood distillate.It includes pre-treatment, distillation and the deoiling step of dalbergia wood medicinal material successively, it is characterised in that：In the deoiling step, it is 7.0~7.5 that regulation control the pH value of distillate, is again heated to 60 DEG C~70 DEG C sealed thermal insulatings 40 minutes, room temperature is cooled to, then it is 5.5~6.0 to adjust pH value, and medicinal carbon is added afterwards, stir well, cool down and filter, obtain final product dalbergia wood distillation liquid product.The preparation of dalbergia wood distillate is carried out using the method, its products obtained therefrom qualification rate is high, and can also simultaneously ensure that the discriminating of ethereal oil composition meets regulation.
Description
Technical field
The invention belongs to processing technique of Chinese herbs field, more particularly to prepare a kind of Chinese medicinal liquor used during Clary injection
A kind of preparation method of preparation intermediate, and in particular to preparation method of dalbergia wood distillate.
Background technology
Clary injection is by dry of the labiate red sage root（That is the red sage root）It is extracted, after purification, distilled with dalbergia wood
After liquid oil removing, it is well mixed, then the processed traditional Chinese medicine injection being made.It has expansion of blood vessels, promotes coronary blood flow
Effect.Clinically it is mainly used in treatment heart line and can be used for the symptoms such as miocardial infarction bitterly, also.
Clary injection standard（WS3-B-3289-98）, record in Traditional Chinese medicine historical preparation the 17th, page 200, and it is fragrant red
Parenteral solution corrigenda letter, pharmacopeia industry hair（2000）No. 13.The process for purification for preparing of dalbergia wood distillate is in its standard：" dalbergia wood adds
Water infiltration, carries out steam distillation, collects distillate about 500ml, refrigerates 24 hours, divides and removes oil reservoir, and the another device of the aqueous solution is collected ".But
Preparation method in the standard has that operability is not strong, and visible foreign matters easily occurs in obtained Clary injection, and sometimes only 88%
The qualification rate of left and right, its qualification rate is low, and there is unstable etc. the technical problem of Clary injection final product quality.Additionally, existing
Preparation method grasp improper, the loss of the distinctive compound such as ethereal oil for being also easy to cause in dalbergia wood distillate.
The content of the invention
It is an object of the invention to provide a kind of preparation method of dalbergia wood distillate, dalbergia wood distillate is carried out using the method
Preparation, its products obtained therefrom qualification rate is high, and can also simultaneously ensure that ethereal oil composition differentiates and meet regulation.
The present invention seeks to what is be achieved through the following technical solutions：
A kind of preparation method of dalbergia wood distillate, it includes pre-treatment, distillation and the deoiling step of dalbergia wood medicinal material successively, its
It is characterised by：In the deoiling step, regulation control distillate pH value be 7.0~7.5, be again heated to 60 DEG C~70 DEG C it is closed
Insulation 40 minutes, is cooled to room temperature, then it is 5.5~6.0 to adjust pH value, and medicinal carbon is added afterwards, stirs well, cools down and mistake
Filter, obtains final product dalbergia wood distillation liquid product.
It is molten particular by the medicinal NaOH for first adding mass percent concentration to be 0.5% in above-mentioned deoiling step
It is 7.0~7.5 that liquid controls the pH value of distillate to adjust, and adds the medicinal hydrochloric acid solution that mass percent concentration is 1% and comes
It is 5.5~6.0 to adjust its pH value.Adjusted by adding medicinal sodium hydroxide solution control distillate pH value have it is following
Effect：First, make distillate in alkalescence condition, and cause that hydro carbons oxidizable under this condition, alcohols material occur oxidation reaction,
Enhancing polarity；2nd, the class material that can aggregate into block or fine shape thing under this condition can be promoted to be reacted, and is polymerized or poly-
Integrated block or fine shape thing, to filter, such as macromolecular alcohol, macromolecular acids；3rd, hydrogen-oxygen is controlled with the scope of control ph
Change the addition of sodium；Because different batches medicinal material obtained in can be reacted with medicinal NaOH in dalbergia wood distillate, and be polymerized or
The water insoluble block of aggregation formation, the content of material of fine shape thing are different；Consumption is very few, is insufficient to allow miscellaneous in distillate
There is fully reaction in matter, cross at most can be in destructive distillation liquid active ingredient.Further heating and thermal insulation can be such that it reacts faster more
Fully, then through subsequent treatment the macromolecular alcohol, the macromolecular acid that remove in distillate are realized.By adding medicinal hydrochloric acid
Solution controls the pH value of distillate to have the effect that to adjust：First, because under the conditions of slant acidity, macromolecule organic acid and
Alcohols material dissolubility is relatively poor；2nd, because under the conditions of slant acidity, activated carbon is to organic acid, the absorption affinity of alcohols material
Preferably, absorption is removed more thoroughly, and pH value is too high or too low to cause the reduction of its adsorption effect.
Used as further optimization, the consumption of above-mentioned medicinal carbon is based on distillate weight 0.05 ‰.If active
Charcoal consumption is not enough, not thorough to generating insoluble substance absorption removing in liquid.If activated carbon dosage is excessive, excessive activity
Charcoal can carry a certain amount of distinctive compound of absorption secretly, cause distinctive compound to lose, and make finished product in identification check, and identification is failed to understand
It is aobvious.
Above-mentioned deoiling step is followed the steps below：Collect equivalent to the 1.2 times of distillations of amount of dalbergia wood medicinal material weight
Liquid, after being refrigerated 12 hours under conditions of 2 DEG C~10 DEG C, extracts equivalent to the 1.1 times of steamings of amount of dalbergia wood medicinal material weight from its bottom
Distillate, filtering, it is 7.0~7.5 to adjust its pH value with the medicinal sodium hydroxide solution that mass percent concentration is 0.5% afterwards, then
60 DEG C~70 DEG C sealed thermal insulatings are heated to after 40 minutes, room temperature is cooled to, then with the medicinal hydrochloric acid that mass percent concentration is 1%
Solution adjustment pH value is 5.5~6.0, add afterwards based on distillate weight 0.05 ‰ amount medicinal carbon, stirring is equal
It is even, be cooled to 2 DEG C~10 DEG C, stand 12 hours, after again from gained distillate bottom extract equivalent to dalbergia wood medicinal material weight
Distillate, through filtering, obtains final product dalbergia wood distillation liquid product.
Used as further optimization, the preparation method of above-mentioned dalbergia wood distillate is specifically followed the steps below：
1st, the pre-treatment of dalbergia wood medicinal material：Dalbergia wood medicinal material is taken, impurity is sorted out and is had the medicinal material that goes mouldy, diameter is ground into through disintegrating machine
For 3mm~6mm is granular or bulk, weigh, cleaning is drained；
2nd, distill：The dalbergia wood medicinal material of gained after draining is taken, is added in multi-function extractor, added equivalent to medicinal material weight 5
The water of amount, is heated to 50 DEG C~60 DEG C again, and closed rear immersion 2.5~3.0 hours is heated and distilled, and is discarded equivalent to medicinal material weight
It is twentieth just after distillate, based on medicinal material weight, 1.2 times of follow-up distillates of amount are collected to being provided with aseptic respirator
In interlayer basin I；
3rd, oil removing：Distillate in interlayer basin I is cooled to 2 DEG C~10 DEG C, and stands 12 hours, after taken out from its bottom
Take equivalent to 1.1 times of distillates of amount of medicinal material weight, two layers of quantitative filter paper and one layer of 0.45 μm of filter membrane mistake are served as a contrast through plate filter
Filter in the interlayer basin II for being provided with aseptic respirator to another, should be extracted from the bottom of interlayer basin I when extracting distillate, and
Note not extracting last oil layer out；Afterwards by medicine that the distillate mass percent concentration in interlayer basin II is 0.5%
It is 7.0~7.5 to adjust pH value with sodium hydroxide solution, is again heated to 60 DEG C~70 DEG C sealed thermal insulatings after 40 minutes, is cooled to room
Temperature, then it is 5.5~6.0 to adjust pH value with the medicinal hydrochloric acid solution that mass percent concentration is 1%, adds press distillate weight afterwards
The medicinal carbon of the amount of the 0.05 ‰ of gauge, stirs, and is cooled to 2 DEG C~10 DEG C, stands 12 hours, after from Sandwich pot
The distillate equivalent to medicinal material weight is extracted in II bottom, and one layer of quantitative filter paper and one layer of 0.22 μm of filter membrane are served as a contrast through plate filter
Filtering, after deliver to it is another be provided with the interlayer basin III of aseptic respirator, obtain final product dalbergia wood distillation liquid product, it is fragrant for preparing
Red parenteral solution.
The present invention has following beneficial effect：
The inventive method carries out the preparation of dalbergia wood distillate, employs specific oil removing impurity-removing method, preferably eliminates
Grease in distillate and the macromolecular alcohols and macromolecular acid that are mixed into, impurity remove effect preferably, also improve medicine
The security of product.Gained dalbergia wood distillate is clear and bright liquid colourless, without obvious opalescence, pH value 5.0~6.0, by fragrant red note
Penetrate liquid standard（WS3-B-3289-98）Standard【Differentiate】(2) method inspection, complies fully with regulation.The red injection of perfume for preparing
Liquid qualification rate is high, steady quality, it is seen that inspection of foreign substance qualification rate is high, and every batch of visible foreign matters qualification rate of Clary injection can be stablized
More than 98.5%, and also it is effectively retained the distinctive compounds such as ethereal oil simultaneously；During storage, being also not in can for medicine
See that inspection of foreign substance is unqualified, improve the stability of medicine.
Specific embodiment
In order to more clearly state the present invention, below the invention will be further described, be depicted below as of the invention
Better embodiment, can not do any limitation to protection scope of the present invention.
Embodiment 1
A kind of preparation method of dalbergia wood distillate, it is specifically what is followed the steps below：
1st, the pre-treatment of dalbergia wood medicinal material：Dalbergia wood medicinal material is taken, impurity is sorted out and is had the medicinal material that goes mouldy, then upper log splitter, powder
It is broken into that diameter about 3mm~4mm is granular or bulk, weighs dalbergia wood medicinal material, upper medicine-washing machine cleaning specifically first cleans one with drinking water
It is secondary, then clean secondary with purified water, clean 2~3 minutes every time, drain；
2nd, distill：The dalbergia wood medicinal material of gained after draining is taken, is added in multi-function extractor, added equivalent to medicinal material weight 5
The purified water of times amount, is heated to 50 DEG C~52 DEG C, it is closed after immersion 2.5 hours, the logical steam heating distillation of interlayer, discard equivalent to
After the twentieth just distillate of medicinal material weight, based on medicinal material weight, the follow-up distillate for collecting 1.2 times of amounts is aseptic to being provided with
In the interlayer basin I of respirator；
3rd, oil removing：The distillate of interlayer basin I is cooled to 2 DEG C~5 DEG C by the cooling water for opening interlayer basin I, and at 2 DEG C
Stand 12 hours under conditions of~5 DEG C, after extracted equivalent to 1.1 times of distillates of amount of medicinal material weight, warp from the bottom of Sandwich pot I
Plate filter serves as a contrast two layers of quantitative filter paper and one layer of 0.45 μm of membrane filtration delivers to another interlayer for being provided with aseptic respirator
In basin II, extracted from the bottom of interlayer basin I when extracting distillate, and note not extracting last oil layer out；Afterwards will folder
Layer basin II in distillate mass percent concentration be 0.5% medicinal sodium hydroxide solution regulation pH value be 7.0~7.2,
60 DEG C~62 DEG C sealed thermal insulatings are again heated to after 40 minutes, room temperature is cooled to, then with the pharmaceutical salts that mass percent concentration is 1%
Acid solution adjustment pH value be 5.5~5.7, add afterwards based on distillate weight 0.05 ‰ amount medicinal carbon, stirring
Uniformly, be then turned on cooling and be water-cooled to 2 DEG C~5 DEG C, and 12 hours are stood under conditions of 2 DEG C~5 DEG C, after from Sandwich pot II
The distillate equivalent to medicinal material weight is extracted in bottom, and one layer of quantitative filter paper and one layer of 0.22 μm of filter membrane mistake are served as a contrast through plate filter
Filter, after deliver to it is another be provided with the interlayer basin III of aseptic respirator, obtain final product dalbergia wood distillation liquid product.
Gained dalbergia wood distillate is clear and bright liquid colourless, without obvious opalescence, pH value 5.0~5.4, by perfume (or spice) in the example
Red parenteral solution standard（WS3-B-3289-98）Standard【Differentiate】(2) method inspection, complies fully with regulation.The dalbergia wood distillate is used
In Clary injection is prepared, the visible foreign matters qualification rate stabilization of Clary injection is more than 98.5%.
Embodiment 2
A kind of preparation method of dalbergia wood distillate, it is specifically what is followed the steps below：
1st, the pre-treatment of dalbergia wood medicinal material：Dalbergia wood medicinal material is taken, impurity is sorted out and is had the medicinal material that goes mouldy, then upper log splitter, powder
It is broken into that diameter about 4mm~6mm is granular or bulk, weighs dalbergia wood medicinal material, upper medicine-washing machine cleaning specifically first cleans one with drinking water
It is secondary, then clean secondary with purified water, clean 2~3 minutes every time, drain；
2nd, distill：The dalbergia wood medicinal material of gained after draining is taken, is added in multi-function extractor, added equivalent to medicinal material weight 5
The purified water of times amount, is heated to 58 DEG C~60 DEG C, it is closed after immersion 3.0 hours, the logical steam heating distillation of interlayer, discard equivalent to
After the twentieth just distillate of medicinal material weight, based on medicinal material weight, the follow-up distillate for collecting 1.2 times of amounts is aseptic to being provided with
In the interlayer basin I of respirator；
3rd, oil removing：The distillate of interlayer basin I is cooled to 8 DEG C~10 DEG C by the cooling water for opening interlayer basin I, and 8
DEG C~10 DEG C under conditions of stand 12 hours, after extracted equivalent to the 1.1 times of distillations of amount of medicinal material weight from the bottom of Sandwich pot I
Liquid, serves as a contrast two layers of quantitative filter paper and one layer of 0.45 μm of membrane filtration delivers to another and be provided with aseptic respirator through plate filter
In interlayer basin II, extracted from the bottom of interlayer basin I when extracting distillate, and note not extracting last oil layer out；Afterwards
By medicinal sodium hydroxide solution that the distillate mass percent concentration in interlayer basin II is 0.5% regulation pH value 7.3~
7.5,68 DEG C~70 DEG C sealed thermal insulatings are again heated to after 40 minutes, it is cooled to room temperature, then with the medicine that mass percent concentration is 1%
With hydrochloric acid solution adjust pH value be 5.7~6.0, add afterwards based on distillate weight 0.05 ‰ amount medicinal carbon,
Stir, be then turned on cooling and be water-cooled to 8 DEG C~10 DEG C, and 12 hours are stood under conditions of 8 DEG C~10 DEG C, after from interlayer
The distillate equivalent to medicinal material weight is extracted in the bottom of tank II, and one layer of quantitative filter paper and one layer of 0.22 μm of filter are served as a contrast through plate filter
Membrane filtration, after deliver to it is another be provided with the interlayer basin III of aseptic respirator, obtain final product dalbergia wood distillation liquid product.
Gained dalbergia wood distillate is clear and bright liquid colourless, without obvious opalescence, pH value 5.5~5.9, by perfume (or spice) in the example
Red parenteral solution standard（WS3-B-3289-98）Standard【Differentiate】(2) method inspection, complies fully with regulation.The dalbergia wood distillate is used
In Clary injection is prepared, the visible foreign matters qualification rate of Clary injection can be made stable more than 98.5%.
Embodiment 3
A kind of preparation method of dalbergia wood distillate, it is specifically what is followed the steps below：
1st, the pre-treatment of dalbergia wood medicinal material：Dalbergia wood medicinal material is taken, impurity is sorted out and is had the medicinal material that goes mouldy, then upper log splitter, powder
It is broken into that diameter about 4mm~5mm is granular or bulk, weighs dalbergia wood medicinal material, upper medicine-washing machine cleaning specifically first cleans one with drinking water
It is secondary, then clean secondary with purified water, clean 2~3 minutes every time, drain；
2nd, distill：The dalbergia wood medicinal material of gained after draining is taken, is added in multi-function extractor, added equivalent to medicinal material weight 5
The purified water of times amount, is heated to 55 DEG C~58 DEG C, it is closed after immersion 2.8 hours, the logical steam heating distillation of interlayer, discard equivalent to
After the twentieth just distillate of medicinal material weight, based on medicinal material weight, the follow-up distillate for collecting 1.2 times of amounts is aseptic to being provided with
In the interlayer basin I of respirator；
3rd, oil removing：The distillate of interlayer basin I is cooled to 5 DEG C~8 DEG C by the cooling water for opening interlayer basin I, and at 5 DEG C
Stand 12 hours under conditions of~8 DEG C, after extracted equivalent to 1.1 times of distillates of amount of medicinal material weight, warp from the bottom of Sandwich pot I
Plate filter serves as a contrast two layers of quantitative filter paper and one layer of 0.45 μm of membrane filtration delivers to another interlayer for being provided with aseptic respirator
In basin II, extracted from the bottom of interlayer basin I when extracting distillate, and note not extracting last oil layer out；Afterwards will folder
Layer basin II in distillate mass percent concentration be 0.5% medicinal sodium hydroxide solution regulation pH value be 7.1~7.4,
65 DEG C~68 DEG C sealed thermal insulatings are again heated to after 42 minutes, room temperature is cooled to, then with the pharmaceutical salts that mass percent concentration is 1%
Acid solution adjustment pH value be 5.6~5.8, add afterwards based on distillate weight 0.05 ‰ amount medicinal carbon, stirring
Uniformly, be then turned on cooling and be water-cooled to 5 DEG C~8 DEG C, and 12 hours are stood under conditions of 5 DEG C~8 DEG C, after from Sandwich pot II
The distillate equivalent to medicinal material weight is extracted in bottom, and one layer of quantitative filter paper and one layer of 0.22 μm of filter membrane mistake are served as a contrast through plate filter
Filter, after deliver to it is another be provided with the interlayer basin III of aseptic respirator, obtain final product dalbergia wood distillation liquid product.
Gained dalbergia wood distillate is clear and bright liquid colourless, without obvious opalescence, pH value 5.3~5.6, by perfume (or spice) in the example
Red parenteral solution standard（WS3-B-3289-98）Standard【Differentiate】(2) method inspection, complies fully with regulation.The dalbergia wood distillate is used
In Clary injection is prepared, the visible foreign matters qualification rate stabilization of Clary injection is more than 98.5%.
Claims (2)
1. a kind of preparation method of dalbergia wood distillate, it is characterised in that：The deoiling step is followed the steps below：Receive
Collect equivalent to 1.2 times of distillates of amount of dalbergia wood medicinal material weight, after being refrigerated 12 hours under conditions of 2 DEG C~10 DEG C, from its bottom
Extract equivalent to 1.1 times of distillates of amount of dalbergia wood medicinal material weight, filtering, afterwards with the medicinal hydrogen that mass percent concentration is 0.5%
It is 7.0~7.5 that sodium hydroxide solution adjusts its pH value, is again heated to 60 DEG C~70 DEG C sealed thermal insulatings after 40 minutes, is cooled to room temperature,
It is 5.5~6.0 to adjust pH value with the medicinal hydrochloric acid solution that mass percent concentration is 1% again, is added afterwards based on distillate weight
0.05 ‰ amount medicinal carbon, stir, be cooled to 2 DEG C~10 DEG C, stand 12 hours, after again from gained distill
The distillate equivalent to dalbergia wood medicinal material weight is extracted in liquid bottom, through filtering, obtains final product dalbergia wood distillation liquid product.
2. the preparation method of dalbergia wood distillate according to claim 1, it is characterised in that it is specifically according to following steps
Carry out：
（1）, dalbergia wood medicinal material pre-treatment：Dalbergia wood medicinal material is taken, impurity is sorted out and is had the medicinal material that goes mouldy, be ground into through disintegrating machine a diameter of
3mm~6mm is granular or bulk, weighs, and cleaning is drained；
（2）, distillation：The dalbergia wood medicinal material of gained after draining is taken, is added in multi-function extractor, added equivalent to 5 times of medicinal material weight
The water of amount, is heated to 50 DEG C~60 DEG C, and closed rear immersion 2.5~3.0 hours, heating distillation is discarded equivalent to medicinal material weight two
After 1/10th first distillate, based on medicinal material weight, 1.2 times of follow-up distillates of amount to the folder for being provided with aseptic respirator are collected
In layer basin I；
（3）, oil removing：Distillate in interlayer basin I is cooled to 2 DEG C~10 DEG C, and stands 12 hours, after extracted from its bottom
Equivalent to 1.1 times of distillates of amount of medicinal material weight, two layers of quantitative filter paper and one layer of 0.45 μm of membrane filtration are served as a contrast through plate filter
Into the interlayer basin II that another is provided with aseptic respirator, should be extracted from the bottom of interlayer basin I when extracting distillate, and not
Last oil layer is extracted out；Afterwards by medicinal hydrogen-oxygen that the distillate mass percent concentration in interlayer basin II is 0.5%
It is 7.0~7.5 to change sodium solution regulation pH value, is again heated to 60 DEG C~70 DEG C sealed thermal insulatings after 40 minutes, is cooled to room temperature, then use
Mass percent concentration be 1% medicinal hydrochloric acid solution adjustment pH value be 5.5~6.0, add afterwards based on distillate weight
The medicinal carbon of 0.05 ‰ amount, stirs, and is cooled to 2 DEG C~10 DEG C, stands 12 hours, after from the bottom of Sandwich pot II
Portion extracts the distillate equivalent to medicinal material weight, and one layer of quantitative filter paper and one layer of 0.22 μm of membrane filtration are served as a contrast through plate filter,
Deliver to afterwards it is another be provided with the interlayer basin III of aseptic respirator, obtain final product dalbergia wood distillation liquid product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242199A (en) * | 1998-07-17 | 2000-01-26 | 张家口市长城制药厂 | Process for producing powder injection of compound red sage root medicine |
| WO2012146596A1 (en) * | 2011-04-26 | 2012-11-01 | OrganoPetroleum PSP AB | Method for removing oil |
| CN202920641U (en) * | 2012-11-09 | 2013-05-08 | 必康制药江苏有限公司 | Xiangdan injection production system |
-
2014
- 2014-07-09 CN CN201410322680.9A patent/CN104027387B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242199A (en) * | 1998-07-17 | 2000-01-26 | 张家口市长城制药厂 | Process for producing powder injection of compound red sage root medicine |
| WO2012146596A1 (en) * | 2011-04-26 | 2012-11-01 | OrganoPetroleum PSP AB | Method for removing oil |
| CN202920641U (en) * | 2012-11-09 | 2013-05-08 | 必康制药江苏有限公司 | Xiangdan injection production system |
Non-Patent Citations (2)
| Title |
|---|
| "香丹注射液超滤工艺的优化研究";王正宽，等。;《中草药》;20131112;第44卷(第21期);第2988-2991页。 * |
| Oil removal from water using biomaterials;Asha Srinivasan et al;《Bioresource Technology 101》;20100316;6594-6600页 * |
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