CN109091650A - A kind of anti-cancer drugs granule and preparation method thereof - Google Patents
A kind of anti-cancer drugs granule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation of anti-cancer drugs granule, include the following steps: that (1) raw material weighs；(2) pretreatment of raw material；(3) extraction is handled；(4) concentration；(5) drying and granulating.The anti-cancer drugs granule that the present invention is finally prepared, material matching is reasonable, and bioavilability is high, has the curative effect of good pre- anti-cancer and treating cancer, and materials safety, great market popularization value.
Description
Technical field
The invention belongs to Chinese materia medica preparation preparation technical fields, and in particular to a kind of anti-cancer drugs granule and its preparation side
Method.
Background technique
With the continuous promotion of modern medical service level, the life and health of people also gets better protection, however cancer
It is still the serious illness for being difficult to subdue, the toxic side effect of chemicotherapy can be mitigated by traditional Chinese medicine cooperation operation, chemicotherapy now,
Promote patient to restore, enhance the tolerance to chemicotherapy, but is not now very significant by the effect of Chinese medicine treating cancer, and
And in the preparation process of Chinese materia medica preparation, using a large amount of Chinese medicine, the content of effective component is very low in final preparation, greatly
Ground causes the waste of resource.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of anti-cancer drugs granule and preparation method thereof is provided,
The anti-cancer drugs granule finally prepared, material matching is reasonable, and bioavilability is high, has good pre- anti-cancer and treatment cancer
The curative effect of disease, and materials safety, great market popularization value.
The present invention is achieved by the following technical solutions:
A kind of preparation of anti-cancer drugs granule, includes the following steps:
(1) raw material weighs:
Weigh 2 ~ 4 parts of paris polyphylla, 2 ~ 4 parts of the uncaria, 4 ~ 6 parts of Fructus Forsythiae, 4 ~ 6 parts of oldenlandia diffusa, full worm 11 ~ 13 of corresponding parts by weight
Part, 4 ~ 6 parts of curcuma zedoary, 2 ~ 4 parts recklessly purple, 3 ~ 5 parts of centipede, 2 ~ 3 parts of semen momordicae it is spare；
(2) pretreatment of raw material:
A. by weighed paris polyphylla, uncaria, Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary, purple Hu, centipede, semen momordicae in step (1)
It putting into deep cooling type pulverizer and is crushed respectively, it is -12 ~ -8 DEG C that the temperature in pulverizer is kept when crushing, pulverization process 20 ~
After 30min, 40 meshes are crossed respectively, then carry out each herb powder after sieving to mix to obtain mixed-powder；
B. it will operate and be impregnated in the investment enzyme solution of mixed-powder obtained in a, temperature when enzyme solution impregnates in holding enzyme solution is
39 ~ 43 DEG C, after 50 ~ 60min of enzyme solution immersion treatment, filter cake and filtrate are filtered to obtain, carries out specific frequency while enzyme solution impregnates
Ultrasonication；
(3) extraction is handled:
Step (1) is operated gained filter cake in b to be placed in soxhlet extraction device, step (1) is operated into filtrate and nothing obtained in b
Water-ethanol carries out mixing and extracts as digestion agent to filter cake, is heated in leaching process using microwave, and microwave heating is protected
Holding the temperature in digestion agent is 88 ~ 94 DEG C, filters to obtain leaching liquor after extracting 10 ~ 12 times repeatedly；
(4) concentration:
Rotary evaporation will be carried out in the leaching liquor investment Rotary Evaporators obtained after extraction processing in step (3), rotary evaporation is straight
Ethanol extract is obtained after to ethyl alcohol evaporating completely；
(5) drying and granulating:
Step (4) resulting ethanol extract is placed in baking oven and is dried, after drying to moisture content is 2 ~ 3%, after drying
It is pelletized in ethanol extract investment granulator.
Further, each ingredient and corresponding parts by weight in enzyme solution in the step (2) operation b are as follows: 2 ~ 3 parts of pectase, fine
It ties up plain 4 ~ 5 parts of enzyme, turn 1 ~ 2 part of glycosides enzyme, 3 ~ 4 parts of nanometer iron powder, 100 ~ 120 parts of deionized water.
Further, the w/v of mixed-powder and enzyme solution is 1g:5 ~ 6mL in step (2) the operation b.
Further, the frequency of ultrasonic wave is 20 ~ 24kHz in step (2) the operation b.
Further, the volume ratio of filtrate and dehydrated alcohol is 1:3 ~ 4 in the step (3).
Further, the frequency of microwave is 12 ~ 14GHz in the step (3).
Further, the revolving speed of Rotary Evaporators is 80 ~ 90rpm in the step (4), when rotary evaporation in water-bath
Temperature setting is 80 ~ 82 DEG C.
Further, temperature control when dry in the step (5) in baking oven is 60 ~ 70 DEG C.
The present invention provides a kind of preparation of anti-cancer drugs granule, selected raw material is all middle medicinal herbs, safety coefficient
Height, for anti-cancer drugs preparation of the invention using Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary as monarch drug in a prescription, centipede, uncaria are ministerial drug, flea
Not, radix bupleuri is adjutant, and semen momordicae is to make medicine, mutual compatibility, and the anti-cancer drugs granule finally prepared is aobvious for the curative effect of cancer
It writes, almost non-toxic side effect.In the preparation process of anti-cancer drugs preparation, raw material is placed in deep cooling type pulverizer carries out first
Pulverization process is crushed under cryogenic conditions, can increase the fineness of crushing, increase the contact area between each raw material, and
The chemical stability of active constituent in Chinese medicine can be ensured to greatest extent, guarantee drug effect, smashed powder is placed in enzyme solution
In impregnated, in enzyme solution of the invention added with cellulase, pectase, turn glycosides enzyme and nanometer iron powder, it is most in
Pharmaceutically active ingredient is present in the protoplast wrapped up by cell wall, and the objects such as cellulose, lignin, pectic substance and hemicellulose
Matter constitutes the compact texture of plant cell wall, it is the main barrier that effective component is suggested from medicinal plant, effectively at
Divide and spread during the extraction process to Extraction medium, by the obstruction of dual resistance cell wall and cytoplasm, selects pectase water
Solve pectic substance and cellulose hydrolyzation cellulose etc., the objects such as pectic substance and cellulose in can degrade cytoplasm and cell wall
Matter reduces the resistance to mass tranfer that mass transfer barrier dissolves out effective component, to accelerate the proposition of effective component, in addition, collocation turns glycosides
Enzyme and nanometer iron powder can reach the dual purpose for effectively proposing object and the non-targeted object dissolution of control in Chinese medicine,
Dissolution efficiency not only is improved, also makes the clarity of extracting solution higher, in enzyme solution processing, ultrasonic wave auxiliary is carried out, due to rubbing
Wiping effect and the absorption of medium etc. make ultrasonic energy be converted into thermal energy, and fuel factor increases the temperature of effective component in Chinese medicine, increase
The solubility of big effective component, improves the leaching rate of effective component.Then it is extracted repeatedly with soxhlet extraction device, further
Extraction rate is improved, during extraction, using microwave heating, effect of the molecule by microwave energy, rotation can be accelerated, if point
Son has certain polarity at this time, then can occur instantaneously to polarize in microwave electromagnetic field, then doing reversal movement velocity is
Hundred million seconds, further the vibration and tearing and interparticle phase mutual friction and collision of generation key, can promote molecular polarity part
It better contacts with and reacts, and a large amount of thermal energy can be generated, so that cell rupture, subsequent cell liquid overflows and is diffused into solvent
In, there is good impetus to the bioavilability of extracting efficiency and raw material.
The present invention has the advantage that compared with prior art
The anti-cancer drugs granule that the present invention is finally prepared, material matching is reasonable, and bioavilability is high, has pre- anti-cancer well
The curative effect of disease and treating cancer, and materials safety, great market popularization value.
Specific embodiment
Embodiment 1
A kind of preparation of anti-cancer drugs granule, includes the following steps:
(1) raw material weighs:
Weigh 2 parts of paris polyphylla, 2 parts of the uncaria, 4 parts of Fructus Forsythiae, 4 parts of oldenlandia diffusa, 11 parts of full worm, 4 parts of curcuma zedoary, purple of corresponding parts by weight
2 parts recklessly, 3 parts of centipede, 2 parts of semen momordicae it is spare；
(2) pretreatment of raw material:
A. by weighed paris polyphylla, uncaria, Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary, purple Hu, centipede, semen momordicae in step (1)
It puts into deep cooling type pulverizer and is crushed respectively, it is -12 DEG C that the temperature in pulverizer is kept when crushing, pulverization process 20min
Afterwards, 40 meshes are crossed respectively, then carry out each herb powder after sieving to mix to obtain mixed-powder；
B. it will operate and be impregnated in the investment enzyme solution of mixed-powder obtained in a, temperature when enzyme solution impregnates in holding enzyme solution is
39 DEG C, after enzyme solution immersion treatment 50min, filter cake and filtrate are filtered to obtain, the ultrasound of specific frequency is carried out while enzyme solution impregnates
Wave processing；
(3) extraction is handled:
Step (1) is operated gained filter cake in b to be placed in soxhlet extraction device, step (1) is operated into filtrate and nothing obtained in b
Water-ethanol carries out mixing and extracts as digestion agent to filter cake, is heated in leaching process using microwave, and microwave heating is protected
Holding the temperature in digestion agent is 88 DEG C, filters to obtain leaching liquor after extracting 10 times repeatedly；
(4) concentration:
Rotary evaporation will be carried out in the leaching liquor investment Rotary Evaporators obtained after extraction processing in step (3), rotary evaporation is straight
Ethanol extract is obtained after to ethyl alcohol evaporating completely；
(5) drying and granulating:
Step (4) resulting ethanol extract is placed in baking oven and is dried, after drying to moisture content is 2%, by the second after drying
It is pelletized in alcohol medicinal extract investment granulator.
Further, each ingredient and corresponding parts by weight in enzyme solution in the step (2) operation b are as follows: 2 ~ 3 parts of pectase, fine
It ties up plain 4 parts of enzyme, turn 1 part of glycosides enzyme, 3 parts of nanometer iron powder, 100 parts of deionized water.
Further, the w/v of mixed-powder and enzyme solution is 1g:5mL in step (2) the operation b.
Further, the frequency of ultrasonic wave is 20kHz in step (2) the operation b.
Further, the volume ratio of filtrate and dehydrated alcohol is 1:3 in the step (3).
Further, the frequency of microwave is 12GHz in the step (3).
Further, the revolving speed of Rotary Evaporators is 80rpm in the step (4), temperature when rotary evaporation in water-bath
Degree is set as 80 DEG C.
Further, temperature control when dry in the step (5) in baking oven is 60 DEG C.
Embodiment 2
A kind of preparation of anti-cancer drugs granule, includes the following steps:
(1) raw material weighs:
Weigh 3 parts of paris polyphylla, 3 parts of the uncaria, 5 parts of Fructus Forsythiae, 5 parts of oldenlandia diffusa, 12 parts of full worm, 5 parts of curcuma zedoary, purple of corresponding parts by weight
3 parts recklessly, 4 parts of centipede, 2.5 parts of semen momordicae it is spare；
(2) pretreatment of raw material:
A. by weighed paris polyphylla, uncaria, Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary, purple Hu, centipede, semen momordicae in step (1)
It puts into deep cooling type pulverizer and is crushed respectively, it is -10 DEG C that the temperature in pulverizer is kept when crushing, pulverization process 25min
Afterwards, 40 meshes are crossed respectively, then carry out each herb powder after sieving to mix to obtain mixed-powder；
B. it will operate and be impregnated in the investment enzyme solution of mixed-powder obtained in a, temperature when enzyme solution impregnates in holding enzyme solution is
41 DEG C, after enzyme solution immersion treatment 55min, filter cake and filtrate are filtered to obtain, the ultrasound of specific frequency is carried out while enzyme solution impregnates
Wave processing；
(3) extraction is handled:
Step (1) is operated gained filter cake in b to be placed in soxhlet extraction device, step (1) is operated into filtrate and nothing obtained in b
Water-ethanol carries out mixing and extracts as digestion agent to filter cake, is heated in leaching process using microwave, and microwave heating is protected
Holding the temperature in digestion agent is 91 DEG C, filters to obtain leaching liquor after extracting 11 times repeatedly；
(4) concentration:
Rotary evaporation will be carried out in the leaching liquor investment Rotary Evaporators obtained after extraction processing in step (3), rotary evaporation is straight
Ethanol extract is obtained after to ethyl alcohol evaporating completely；
(5) drying and granulating:
Step (4) resulting ethanol extract is placed in baking oven and is dried, after drying to moisture content is 2.5%, after drying
It is pelletized in ethanol extract investment granulator.
Further, each ingredient and corresponding parts by weight in enzyme solution in the step (2) operation b are as follows: 2.5 parts of pectase, fine
It ties up plain 4.5 parts of enzyme, turn 1.5 parts of glycosides enzyme, 3.5 parts of nanometer iron powder, 110 parts of deionized water.
Further, the w/v of mixed-powder and enzyme solution is 1g:5.5mL in step (2) the operation b.
Further, the frequency of ultrasonic wave is 22kHz in step (2) the operation b.
Further, the volume ratio of filtrate and dehydrated alcohol is 1:3.5 in the step (3).
Further, the frequency of microwave is 13GHz in the step (3).
Further, the revolving speed of Rotary Evaporators is 85rpm in the step (4), temperature when rotary evaporation in water-bath
Degree is set as 81 DEG C.
Further, temperature control when dry in the step (5) in baking oven is 65 DEG C.
Embodiment 3
A kind of preparation of anti-cancer drugs granule, includes the following steps:
(1) raw material weighs:
Weigh 4 parts of paris polyphylla, 4 parts of the uncaria, 6 parts of Fructus Forsythiae, 6 parts of oldenlandia diffusa, 13 parts of full worm, 6 parts of curcuma zedoary, purple of corresponding parts by weight
4 parts recklessly, 5 parts of centipede, 3 parts of semen momordicae it is spare；
(2) pretreatment of raw material:
A. by weighed paris polyphylla, uncaria, Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary, purple Hu, centipede, semen momordicae in step (1)
It puts into deep cooling type pulverizer and is crushed respectively, it is -8 DEG C that the temperature in pulverizer is kept when crushing, pulverization process 30min
Afterwards, 40 meshes are crossed respectively, then carry out each herb powder after sieving to mix to obtain mixed-powder；
B. it will operate and be impregnated in the investment enzyme solution of mixed-powder obtained in a, temperature when enzyme solution impregnates in holding enzyme solution is
43 DEG C, after enzyme solution immersion treatment 60min, filter cake and filtrate are filtered to obtain, the ultrasound of specific frequency is carried out while enzyme solution impregnates
Wave processing；
(3) extraction is handled:
Step (1) is operated gained filter cake in b to be placed in soxhlet extraction device, step (1) is operated into filtrate and nothing obtained in b
Water-ethanol carries out mixing and extracts as digestion agent to filter cake, is heated in leaching process using microwave, and microwave heating is protected
Holding the temperature in digestion agent is 94 DEG C, filters to obtain leaching liquor after extracting 12 times repeatedly；
(4) concentration:
Rotary evaporation will be carried out in the leaching liquor investment Rotary Evaporators obtained after extraction processing in step (3), rotary evaporation is straight
Ethanol extract is obtained after to ethyl alcohol evaporating completely；
(5) drying and granulating:
Step (4) resulting ethanol extract is placed in baking oven and is dried, after drying to moisture content is 3%, by the second after drying
It is pelletized in alcohol medicinal extract investment granulator.
Further, each ingredient and corresponding parts by weight in enzyme solution in the step (2) operation b are as follows: 3 parts of pectase, fiber
5 parts of plain enzyme turns 2 parts of glycosides enzyme, 4 parts of nanometer iron powder, 120 parts of deionized water.
Further, the w/v of mixed-powder and enzyme solution is 1g:6mL in step (2) the operation b.
Further, the frequency of ultrasonic wave is 24kHz in step (2) the operation b.
Further, the volume ratio of filtrate and dehydrated alcohol is 1:4 in the step (3).
Further, the frequency of microwave is 14GHz in the step (3).
Further, the revolving speed of Rotary Evaporators is 90rpm in the step (4), temperature when rotary evaporation in water-bath
Degree is set as 82 DEG C.
Further, temperature control when dry in the step (5) in baking oven is 70 DEG C.
Comparative example 1
This comparative example 1 compared with Example 2, saves the ultrasonication in step (2) operation b, method step in addition to this
It is rapid all the same.
Comparative example 2
This comparative example 2 compared with Example 2, saves the whole operation of step (2) operation b, and method and step in addition to this is equal
It is identical.
Comparative example 3
Microwave heating in step (3) compared with Example 2, is melted into conventional heating water bath, in addition to this by this comparative example 3
Method and step it is all the same.
Control group
Commercially available common Traditional Chinese Drug Anticancer new drug granule.
In order to compare effect of the present invention, embodiment 2, comparative example 1, comparative example 2, comparative example 3 are used respectively
Method preparation anti-cancer drugs granule and the anti-cancer drugs granule of control group carry out external inhibiting tumor assay, specific experiment
It is:
(1) culture of tumour cell:
Human cervical carcinoma Hela cell's strain DMEM culture solution culture for containing 10% fetal calf serum is chosen, condition of culture is 3 DEG C, 5%CO2
Concentration and saturated humidity.When cell grows to logarithmic growth phase, with 25% trypsin digestion cell, dispels cell and be diluted to
106/ mL, every 100 μ L of hole are inoculated in 96 orifice plates, in case MTT experiment.
(2) cell proliferation experiment (mtt assay)
With the DMEM solution containing 10% fetal calf serum by embodiment 2, comparative example 1, comparative example 2, comparative example 3, right
It is diluted to the solution that concentration is 25 μ g/mL according to the anti-cancer drugs granule of group, every 100 μ L of hole is inoculated in 96 orifice plates, is put into culture
Case continues culture 16,32,48h.5 μ L of 5mg/mL MTT solution is added in every hole, continues to cultivate 5h, measures every hole absorbance.With not
The culture cell for adding any processing is blank control.Each processing is respectively provided with 12 parallel groups, calculates separately cell inhibitory rate.
Specific experiment correlation data is as shown in table 1 below:
Table 1
| Cultivate 16h inhibiting rate % | Cultivate 32h inhibiting rate % | Cultivate 48h inhibiting rate % | |
| Embodiment 2 | 13±1.9 | 15±1.8 | 16±2.1 |
| Comparative example 1 | 12±1.6 | 13±1.5 | 15±1.6 |
| Comparative example 2 | 9±1.2 | 11±1.5 | 12±1.4 |
| Comparative example 3 | 11±1.3 | 13±1.5 | 13±1.4 |
| Control group | 10±1.2 | 11±1.3 | 12±1.2 |
Note: inhibiting rate=1-(experimental group absorbance values/blank control group absorbance values described in upper table 1) ×
100%。
The anti-cancer drugs granule that the present invention is finally prepared it can be seen from upper table 1, material matching is reasonable, biological utilisation
Degree is high, the curative effect of the pre- anti-cancer having had and treating cancer, and materials safety, great market popularization value.
Claims (8)
1. a kind of preparation of anti-cancer drugs granule, which comprises the steps of:
(1) raw material weighs:
Weigh 2 ~ 4 parts of paris polyphylla, 2 ~ 4 parts of the uncaria, 4 ~ 6 parts of Fructus Forsythiae, 4 ~ 6 parts of oldenlandia diffusa, full worm 11 ~ 13 of corresponding parts by weight
Part, 4 ~ 6 parts of curcuma zedoary, 2 ~ 4 parts recklessly purple, 3 ~ 5 parts of centipede, 2 ~ 3 parts of semen momordicae it is spare；
(2) pretreatment of raw material:
A. by weighed paris polyphylla, uncaria, Fructus Forsythiae, oldenlandia diffusa, full worm, curcuma zedoary, purple Hu, centipede, semen momordicae in step (1)
It putting into deep cooling type pulverizer and is crushed respectively, it is -12 ~ -8 DEG C that the temperature in pulverizer is kept when crushing, pulverization process 20 ~
After 30min, 40 meshes are crossed respectively, then carry out each herb powder after sieving to mix to obtain mixed-powder；
B. it will operate and be impregnated in the investment enzyme solution of mixed-powder obtained in a, temperature when enzyme solution impregnates in holding enzyme solution is
39 ~ 43 DEG C, after 50 ~ 60min of enzyme solution immersion treatment, filter cake and filtrate are filtered to obtain, carries out specific frequency while enzyme solution impregnates
Ultrasonication；
(3) extraction is handled:
Step (1) is operated gained filter cake in b to be placed in soxhlet extraction device, step (1) is operated into filtrate and nothing obtained in b
Water-ethanol carries out mixing and extracts as digestion agent to filter cake, is heated in leaching process using microwave, and microwave heating is protected
Holding the temperature in digestion agent is 88 ~ 94 DEG C, filters to obtain leaching liquor after extracting 10 ~ 12 times repeatedly；
(4) concentration:
Rotary evaporation will be carried out in the leaching liquor investment Rotary Evaporators obtained after extraction processing in step (3), rotary evaporation is straight
Ethanol extract is obtained after to ethyl alcohol evaporating completely；
(5) drying and granulating:
Step (4) resulting ethanol extract is placed in baking oven and is dried, after drying to moisture content is 2 ~ 3%, after drying
It is pelletized in ethanol extract investment granulator.
2. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that in step (2) the operation b
Each ingredient and corresponding parts by weight in enzyme solution are as follows: 2 ~ 3 parts of pectase, turns 1 ~ 2 part of glycosides enzyme, nanometer iron powder 3 ~ 4 at 4 ~ 5 parts of cellulase
Part, 100 ~ 120 parts of deionized water.
3. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that in step (2) the operation b
The w/v of mixed-powder and enzyme solution is 1g:5 ~ 6mL.
4. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that in step (2) the operation b
The frequency of ultrasonic wave is 20 ~ 24kHz.
5. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that filtrate in the step (3)
Volume ratio with dehydrated alcohol is 1:3 ~ 4.
6. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that microwave in the step (3)
Frequency be 12 ~ 14GHz.
7. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that rotation in the step (4)
The revolving speed of evaporimeter is 80 ~ 90rpm, and temperature setting when rotary evaporation in water-bath is 80 ~ 82 DEG C.
8. a kind of preparation of anti-cancer drugs granule according to claim 1, which is characterized in that dry in the step (5)
When baking oven in temperature control be 60 ~ 70 DEG C.
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Citations (3)
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|---|---|---|---|---|
| CN102475822A (en) * | 2010-11-27 | 2012-05-30 | 冯文明 | Oral liquid capable of preventing and treating cervical cancer |
| CN104415290A (en) * | 2013-08-26 | 2015-03-18 | 广东省中医院 | Stagnation-removing decoction oral liquid and preparation method thereof |
| CN107335022A (en) * | 2017-07-27 | 2017-11-10 | 冯敏杰 | A kind of compound zedoary bark of eucommia anti-cervical cancer oral liquid and its preparation technology |
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2018
- 2018-10-10 CN CN201811175823.2A patent/CN109091650A/en active Pending
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|---|---|---|---|---|
| CN102475822A (en) * | 2010-11-27 | 2012-05-30 | 冯文明 | Oral liquid capable of preventing and treating cervical cancer |
| CN104415290A (en) * | 2013-08-26 | 2015-03-18 | 广东省中医院 | Stagnation-removing decoction oral liquid and preparation method thereof |
| CN107335022A (en) * | 2017-07-27 | 2017-11-10 | 冯敏杰 | A kind of compound zedoary bark of eucommia anti-cervical cancer oral liquid and its preparation technology |
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