CN103169912A - Improvement for preparation method of Chinese material medical preparation for treating primary hepatic carcinoma - Google Patents
Improvement for preparation method of Chinese material medical preparation for treating primary hepatic carcinoma Download PDFInfo
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- CN103169912A CN103169912A CN2011104312672A CN201110431267A CN103169912A CN 103169912 A CN103169912 A CN 103169912A CN 2011104312672 A CN2011104312672 A CN 2011104312672A CN 201110431267 A CN201110431267 A CN 201110431267A CN 103169912 A CN103169912 A CN 103169912A
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Abstract
The invention relates to an improvement for a preparation method of a Chinese material medical preparation for treating primary hepatic carcinoma, the Chinese material medical preparation comprises the following raw materials: Codonopsis pilosula, white atractylodes rhizome, ground beeltle, Sculellaria barbata, semen coicis, oyster, rhizoma cyperi, turtle shell, Astragalus mongholicus, rheum officinale, herba patriniae, radix curcumae, oriental wormwood, capillary Artemisia, agilawood, Paris polyphylla, pericarpium citri reticulatae, Poria cocos, Sappan Wood, caulis clematidis armandii, peach kernel and radix bupleuri; agilawood fine powder employs a superfine crushing method on the basis of a traditional preparation method, a drying process employs microwave vacuum drying. The problems of incompletely extraction of effective constituents, low solubility of the agilawood fine powder, storage of traditional Chinese medicine volatile oil, drying of volatile organic constituents, so that the bioavailability of the preparation is increased.
Description
Technical field
The present invention relates to a kind of improvement of compound Chinese medicinal preparation preparation method, the preparation method that particularly relates to the gan fu le preparation is improved.
Background technology
Chinese traditional compound medicine---" gan fu le " is comprised of Radix Codonopsis, the Rhizoma Atractylodis Macrocephalae, Eupolyphaga Seu Steleophaga, Herba Scutellariae Barbatae, Semen Coicis, Concha Ostreae, Rhizoma Cyperi, Carapax Trionycis, the Radix Astragali, Radix Et Rhizoma Rhei, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Lignum Aquilariae Resinatum, Rhizoma Paridis, Pericarpium Citri Reticulatae, Poria, Lignum Sappan, Caulis Clematidis Armandii, Semen Persicae and Radix Bupleuri Chinese medicine, have that spleen invigorating is regulated the flow of vital energy, blood stasis dispelling softening the hard mass, heat-clearing toxin-expelling functions, be applicable to treat take the insufficiency of the spleen primary hepatocarcinoma as main symptom of the liver stasis of blood.Publication number is to disclose traditional preparation technology in the application documents of CN 1644213, CN1593523: in leaching process, the volatile oil yield is not high, and dry run adopts cold drying (spray drying method), and volatile oil component is volatile.
The present invention has successfully solved the high efficiency extraction volatile ingredient on the prior art basis, the not volatile difficult problem of volatile oil component dry run, thus improved the bioavailability of said preparation.
Summary of the invention
improved preparation technology: accurately take the clean medical material of pulverizing and extracting by recipe quantity, Lignum Aquilariae Resinatum half amount is ground into fine powder, remaining Lignum Aquilariae Resinatum, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Rhizoma Cyperi, Radix Bupleuri adds 10 times of water gagings and soaked 1.5 hours, vapor distillation extracted volatile oil in 6 hours, with beta-schardinger dextrin-(beta-schardinger dextrin-(g): 50 ℃ of enclose of volatilization oil mass (ml)=5:1) 1 hour, 40 ℃ are dried to dried, standby, the another device splendid attire of distillate, 13 flavors such as medicinal residues and all the other Radix Codonopsis add 8 times of water gagings of water and decoct twice, 2 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, aqueous solution after filtrate and above-mentioned distillation merges, being concentrated into relative density is the clear paste of 1.10 (80 ℃), add ethanol to make containing amount of alcohol is 50%, stir evenly, cold preservation 24 hours, get supernatant and reclaim ethanol, being condensed into relative density is 1.25～1.30(80 ℃) thick paste, vacuum drying (vacuum-0.05～-0.1MPa, 60～70 ℃), pulverize, add above-mentioned clathrate and Lignum Aquilariae Resinatum fine powder, mixing, with 85% ethanol granulation.
Specific embodiment
One, optimum extraction process determines
Select the volatile oil of the 8 flavor medical materials such as extraction by steam distillation Lignum Aquilariae Resinatum, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Rhizoma Cyperi, Radix Bupleuri.Through Preliminary experiment results and bibliographical information, volatile oil is extracted 3 kinds of larger factors of impact: soak time, amount of water, return time is investigated, and each factor is got 3 levels.Get Lignum Aquilariae Resinatum 55.5g, Rhizoma Atractylodis Macrocephalae 554g, Pericarpium Citri Reticulatae 554g, Herba Patriniae 554g, Radix Curcumae 554g, Herba Artemisiae Scopariae 554g, Rhizoma Cyperi 554g, Radix Bupleuri 277g in the prescription ratio, under the operation repetitive condition, according to (L
9(3)
4) listed orthogonal table carries out orthogonal test, separates volatile oil, and is standby after anhydrous sodium sulfate dehydration.Take the volatile oil total amount as investigating index, carry out comprehensive grading, preferred optimum extraction process.
The analysis of variance table that table 1 volatile oil must be measured
| Soruces of variation | Sum of squares of deviations | The free degree | Variance | The F value | Conspicuousness |
| A | 0.858 | 2 | 0.0046 | 11.440 | P<0.05 |
| B | 0.543 | 2 | 0.0028 | 7.240 | P>0.05 |
| C | 1.419 | 2 | 0.0074 | 18.920 | P<0.05 |
| Error | 0.07 | 2 | 0.035 |
F
0.1（2，2）=9，F
0.25（2，2）=19
Conclusion: consider with volatile oil total amount R value and intuitive analysis result, each factor effect primary and secondary is C＞A＞B, and optimised process is A
3B
2C
3Variance analysis shows that (data see Table 1): A, C factor have significant difference, and the B factor is not had a significant difference, desirable any level.Therefore consider that extraction process is with A
3B
1C
3Be the best.Namely get 8 kinds of medical materials such as Lignum Aquilariae Resinatum, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Rhizoma Cyperi, Radix Bupleuri and add 10 times of water gagings immersions 1.5 hours, vapor distillation extracted 6 hours.
Two, the research of clathrate process
The primary election of enclose condition
Affecting the inclusion essential oil factor has: beta-schardinger dextrin--volatilization oil mass is than (g:ml), the enclose temperature (℃), the enclose time (hour).Therefore, adopt uniform design to carry out primary election to the enclose condition, factor and level are: beta-schardinger dextrin--volatilization oil mass is than 2:1～8:1, and 20～50 ℃ of enclose temperature, enclose time 30～120min list even table U in
7(7
6) U in table
7(7
3) table.
Adopt saturated water solution method: test according to even table conditional, get beta-schardinger dextrin-, add water 100ml and make dissolving, add volatile oil 1ml(1ml ethanol dilution), stir and carried out enclose in 1 hour, cold preservation below 4 ℃ 24 hours, filter, filter cake washes away not inclusion volatile oil with a small amount of ether.40 ℃ of dryings are weighed, and get clathrate amount (g).
Above-mentioned clathrate is added water 100ml, and steam distillation 6 hours reads volatile oil volume (ml), is calculated as follows inclusion rate.
Table 2, inclusion essential oil result
| Tested number | A | B | C | Inclusion rate (%) | Recovery rate (%) |
| 1 | 1（2：1） | 2（25） | 3（60） | 50 | 88 |
| 2 | 2（3：1） | 4（35） | 6（105） | 76 | 87 |
| 3 | 3（4：1） | 6（45） | 2（45） | 80 | 93 |
| 4 | 4（5：1） | 1（20） | 5（90） | 75 | 79 |
| 5 | 5（6：1） | 3（30） | 1（30） | 80 | 75 |
| 6 | 6（7：1） | 5（40） | 4（75） | 80 | 72 |
| 7 | 7（8：1） | 7（50） | 7（120） | 70 | 63 |
By above result, inclusion rate is done Multivariate Linear and return, gained linear equations Y=-61.6A+0.04B-0.08C+90.7, F=1.03 tables look-up and knows: F
0.1(3,3)=5.27, therefore, gained regression equation linearity is not good.But inclusion rate is with the situation of each factors vary as can be known due to above result, and namely A beta-schardinger dextrin--volatilization oil mass is than being 4:1～6:1; 30～50 ℃ of B enclose temperature; Change the gained inclusion rate in 0.5 hour～1.5 hours C enclose time scope higher.Consider that the factor that affects inclusion rate still has baking temperature (D).Therefore, according to the situation of above-mentioned inclusion rate with each factors vary, design orthogonal test, preferred best enclose condition.
The empirical factor water-glass sees Table 3, and experimental result sees Table 4-table 6.
Table 3, factor level table
| Factor | A（g：ml） | B（℃） | C（min） | D（℃） |
| 1 | 4：1 | 30 | 30 | 30 |
| 2 | 5：1 | 40 | 60 | 40 |
| 3 | 6：1 | 50 | 90 | 50 |
Table 4, orthogonal test scheme and table as a result
Table 5, inclusion rate analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean | The free degree | All square | The F value | Conspicuousness |
| A | 104 | 2 | 52 | 52 | P<0.05 |
| B | 62 | 2 | 31 | 31 | P<0.05 |
| C | 50 | 2 | 25 | 25 | P<0.05 |
| |
2 | 2 | 1 | ||
| |
2 | 2 | 1 |
F
0。05（2，2）= 19.00 F
0。01（2，2）= 99.00
Table 6, recovery rate analysis of variance table
| Soruces of variation | Sum of sguares of deviation from mean | The free degree | All square | The F value | Conspicuousness |
| A | 344 | 2 | 172 | 49 | P<0.05 |
| B | 46 | 2 | 23 | 6.6 | P>0.05 |
| C | 7 | 2 | 3.5 | 1 | P>0.05 |
| D | 7 | 2 | 3.5 | ||
| Error e | 7 | 2 | 3.5 |
F
0。05（2，2）= 19.00 F
0。01（2，2）= 99.00
By the intuitive analysis of inclusion rate and R value as can be known, the factor size that affects result is followed successively by A＞B＞C＞D, and from variance analysis, factor A, B, C have the significance impact, therefore optimum process condition is A
2B
3C
2D
2
By the intuitive analysis of recovery rate and R value as can be known, the factor size that affects result is followed successively by A＞B＞C＞D, from variance analysis, and the impact of factor A tool significance, B, C there are no significant impact is A therefore select optimum process condition
1B
2C
3D
2
By technique as can be known, inclusion rate is important than recovery rate, is A therefore select optimum process condition
2B
3C
2D
2, namely beta-schardinger dextrin-is 5:1 with volatilization oil mass ratio, 50 ℃ of enclose 60min, and 40 ℃ are dried to dried.
Three, drying condition research
If clear paste is excess Temperature in dry run, might the quality of finished product be impacted.For this reason, take the contained content of hesperidin of dried dried cream powder as investigating index, the impact on drying effect under normal pressure is investigated on different baking temperatures.The results are shown in Table 7.
The impact of the baking temperature drying effect that table 7 is different
| Temperature (℃) | Content of hesperidin (mg/g) |
| 60～70 | 2.48 |
| 70～80 | 2.45 |
| 80～90 | 2.44 |
From upper table result, along with the rising of baking temperature, the contained content of hesperidin of dried dried cream powder slightly has reduction, but impact is not too obvious.Consider in dry run, the medicine heating temperature is more low better, more is conducive to ensure effective constituent and can not be destroyed.Therefore baking temperature is defined as 60～70 ℃.
The impact of different vacuum on drying effect
Under the condition of 60～70 ℃ of baking temperatures, adopt different vacuum that drying effect is investigated, the results are shown in Table 8.
The impact on drying effect of table 8, different vacuum
| Vacuum | Drying time (h) | Moisture content | Content of hesperidin (mg) |
| －0.1～－0.5 |
12 | 2.9 | 42.5 |
| －0.05～－0.1MPa | 9 | 2.7 | 42.4 |
| －0.01～－0.05MPa | 6 | 2.7 | 42.7 |
Upper table shows, from moisture content and dry after the contained Hesperidin amount of fine powder, different vacuum is little on the result impact, but from drying time, vacuum is larger, required drying time is shorter, but higher to equipment requirements simultaneously.Consider, select vacuum be-0.05～-0.1MPa, 60～70 ℃ of 9 hours lower drying times of condition.
Four, content of hesperidin detects
Chromatographic column: C18(Kromasil 5 μ m 250 mm * 4.6 mm); Mobile phase: methanol-4% acetum (25: 75); Detect wavelength: 284 nm; Flow velocity: 1.0 ml/min; Column temperature: room temperature.Under selected condition, in Hesperidin peak and sample, other component chromatographic peak can reach baseline separation, and chromatographic peak separating degree adjacent with other is greater than 1.5; Press Hesperidin peak calculating, number of theoretical plate is more than 2000.
The sample solution preparation
The preparation precision of reference substance solution takes Hesperidin reference substance 5mg, puts in the 50ml measuring bottle, adds methanol and makes dissolving, and be diluted to scale, shakes up.The accurate 5ml that draws puts in the 25ml measuring bottle, adds methanol and is diluted to scale, shakes up, and namely gets the Hesperidin reference substance solution that approximately contains 0.02mg in every 1ml.
The need testing solution preparation method: get approximately 0.5g of this product content, be ground into fine powder, accurately weighed, put in tool plug conical flask, precision adds methanol 50ml, and weighed weight was put in water-bath reflux 2 hours, let cool, weighed weight, add the weight that methanol is supplied less loss again, shakes up, filter, get subsequent filtrate and namely get need testing solution.
All the other the recipe quantity medical materials except Pericarpium Citri Reticulatae are got in the preparation of negative sample solution, press the negative sample that the process of preparing preparation lacks Pericarpium Citri Reticulatae, make the negative solution of Pericarpium Citri Reticulatae by above-mentioned need testing solution preparation method.
The specificity testGet reference substance solution, need testing solution and negative blank sample solution, difference sample introduction 10 μ l, record chromatogram under above-mentioned chromatographic condition, the results are shown in Figure 1-Fig. 3.Known by chromatogram, in the need testing solution chromatograph, with Hesperidin reference substance chromatographic peak relevant position on respective peaks is arranged, and in negative solution chromatograph without this peak, illustrate negative noiseless.
Sample determinationMeasure the content of Hesperidin in ten batch samples by above-mentioned content assaying method, the average content of ten batches of finished products is about 0.74 mg/ grain, and content all meets the requirements.
Claims (3)
1. a preparation method for the treatment of the primary hepatocarcinoma Chinese medicine preparation is improved, and described compound Chinese medicinal preparation is comprised of Radix Codonopsis, the Rhizoma Atractylodis Macrocephalae, Eupolyphaga Seu Steleophaga, Herba Scutellariae Barbatae, Semen Coicis, Concha Ostreae, Rhizoma Cyperi, Carapax Trionycis, the Radix Astragali, Radix Et Rhizoma Rhei, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Lignum Aquilariae Resinatum, Rhizoma Paridis, Pericarpium Citri Reticulatae, Poria, Lignum Sappan, Caulis Clematidis Armandii, Semen Persicae and Radix Bupleuri, preparation process comprises: above 20 simply, Lignum Aquilariae Resinatum half amount is ground into fine powder, remaining Lignum Aquilariae Resinatum, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Rhizoma Cyperi, Radix Bupleuri adds suitable quantity of water and soaks, vapor distillation extracts volatile oil, use beta-cyclodextrin inclusion compound, dry, standby, the another device of distillate is collected, 13 flavors such as medicinal residues and all the other Radix Codonopsis decoct with water twice, collecting decoction, filter, aqueous solution after filtrate and above-mentioned distillation merges, be concentrated into the clear paste that relative density is, add ethanol, stir evenly, cold preservation, get supernatant and reclaim ethanol, be condensed into thick paste, dry, pulverize, add above-mentioned clathrate and Lignum Aquilariae Resinatum fine powder, mixing, granulate, dry, incapsulate, and get final product,
It is characterized in that: the volatile oil component leaching process is that Lignum Aquilariae Resinatum, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Herba Patriniae, Radix Curcumae, Herba Artemisiae Scopariae, Rhizoma Cyperi, Radix Bupleuri 8 flavor medical materials are put into multifunctional extracting pot, add water soaking 1-3 hour that 8-10 doubly measures, extracted volatile oil in vapor distillation 4-8 hour, the another device of distillate is collected, and is standby; Other composition leaching process is with all the other 13 flavor medical materials such as Radix Codonopsis, and medicinal residues and every part of medical material after extraction volatile oil decoct with water twice, and 1.5-4 hour for the first time, 1-3 hour for the second time, amount of water was 8-10 doubly, filters collecting decoction.
2. a kind of preparation method for the treatment of the primary hepatocarcinoma Chinese medicine preparation is improved according to claim 1, and it is characterized in that: dry run adopts the microwave vacuum drying method, vacuum :-0.08～-0.1MPa, temperature: 60～70 ℃.
3. a kind of preparation method for the treatment of the primary hepatocarcinoma Chinese medicine preparation is improved according to claim 1, and it is characterized in that: the clathrate process parameter is: beta-schardinger dextrin-is 5:1 with volatilization oil mass ratio, 50 ℃ of enclose 60min, and 40 ℃ are dried to dried.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696489A (en) * | 2017-10-24 | 2019-04-30 | 汉寿康运医药科技有限公司 | A kind of finger-print of gan fu le preparation |
| CN111388622A (en) * | 2018-12-14 | 2020-07-10 | 康普药业股份有限公司 | Ganfule capsule preparation |
-
2011
- 2011-12-21 CN CN2011104312672A patent/CN103169912A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696489A (en) * | 2017-10-24 | 2019-04-30 | 汉寿康运医药科技有限公司 | A kind of finger-print of gan fu le preparation |
| CN109696489B (en) * | 2017-10-24 | 2023-12-08 | 汉寿康运医药科技有限公司 | Preparation method of fingerprint of Ganfule preparation |
| CN111388622A (en) * | 2018-12-14 | 2020-07-10 | 康普药业股份有限公司 | Ganfule capsule preparation |
| CN111388622B (en) * | 2018-12-14 | 2022-12-02 | 康普药业股份有限公司 | Ganfule capsule preparation |
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Application publication date: 20130626 |