CN102641302B - A kind of method improving Chinese medicine extract extract powder softening point - Google Patents
A kind of method improving Chinese medicine extract extract powder softening point Download PDFInfo
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Abstract
The invention discloses a kind of method that can improve Chinese medicine extract extract powder softening point, it is characterized in that adding appropriate composite auxiliary material in the Chinese medicine extraction concentrated solution that softening point is low, is this composite auxiliary material by plasdone? S-630, light magnesium oxide, maltodextrin form, stirring makes it dispersed, will can obtain the higher extractum powder of softening point after concentrated solution drying.Advantage of the present invention is as follows: 1) the inventive method is simple, and only need add a small amount of composite auxiliary material in extract concentration process, composite auxiliary material dissolubility is good, substantially can not extend the production time; 2) contained in composite auxiliary material various adjuvants are preparation and commonly use adjuvant, take rear avirulence and untoward reaction; 3) adjuvant addition is few, improves the compliance of patient, cheap, maximizedly reduces production cost; 4) this composite auxiliary material not only can improve the softening point of material, has protection against the tide, taste masking simultaneously, improves the features such as Chinese medicine preparation raw material mobility, facilitates the preparation of preparation and improves the quality of the pharmaceutical preparations.
Description
(1) technical field
The present invention relates to field of traditional Chinese, be specifically related to a kind of method improving Chinese medicine extract extract powder softening point.
(2) background technology
For non-crystal material, the transformation of solid-liquid be one by progressive formation that is softening and then melting, the transition temperature that neither one is determined, therefore draws the concept of " softening point ".Softening point is commonly used to the solid-liquid transformation critical temperature characterizing noncrystal material, usually adopts Vicat softening point tester to measure.
The noncrystal mixture that the preparation raw material of Chinese medicine compound or single preparations of ephedrine is generally all made up of tens kinds of even hundreds of materials, therefore softening point is a build-in attribute of Chinese medicine preparation raw material.At present, although rarely have report to the research of Chinese medicine preparation raw material softening point, softening point is the key factor affecting production process and product quality really in process of production.Such as, for the low-down Chinese medicine preparation raw material of some softening point, a small amount of heat is created in the process of dry granulation roller extruding, rise in temperature and only immediately ruckbildung occurs after 5-6 DEG C, softening preparation raw material cannot form the plate object with certain degree of hardness, thus cannot prepare granule; And for example in wet-granulation process, preparation raw material needs after being prepared into soft material to adopt oscillating granulator to prepare granule, and producing ruckbildung by during screen cloth due to extruding, causing preparation raw material to be all attached on screen cloth cannot granulate; For another example, in tablet manufacture, the preparation raw material that softening point is lower under the effect of upper and lower stamping press can cause sticking etc. because of softening, and can say, existing preparation technique is nearly all difficult to Chinese medicine preparation bulk formulation low for softening point to be shaped.
In addition, due to the complicated component of Chinese medicine preparation raw material, the research of the Chinese medicine extract material base of some compound recipe or folk prescription imperfection, the material therefore utilizing various separation method to remove softening point in extract low is simply theoretically unsound.
In current production process, often adopt the method for adding a large amount of adjuvant to improve its preparation formability when running into the low Chinese medicine preparation raw material of softening point, the addition of adjuvant can account for 80% of prescription sometimes.Although this method has certain effect, cost is also very large.After Chinese medicine extract is dried to extract powder, single dose is natively larger, if add a large amount of adjuvant again, be easy to occur that single is taken more than 5, tablet or takes granule 12g with the preparation of first-class heavy dose, this can reduce the compliance of patient greatly.In addition, add the production cost that a large amount of adjuvant also can increase enterprise greatly, reduce economic benefit.Therefore, under being badly in need of a kind of prerequisite not changing preparation raw material composition, only add the method that a small amount of adjuvant just can significantly improve preparation raw material.
(3) summary of the invention
Technical problem to be solved by this invention is the softening point by selecting suitable pharmaceutic adjuvant to improve preparation raw material, requires that supplementary product consumption is few, simultaneously noiseless to the release of drug main composition; The method answers favorable reproducibility.
For solving the problem, technical scheme of the present invention is as follows:
Improve a method for Chinese medicine preparation raw material softening point, it is characterized in that adding appropriate composite auxiliary material in the Chinese medicine extraction concentrated solution that softening point is low, stir and make it dispersed, will can obtain the higher extractum powder of softening point after concentrated solution drying.
Above-mentioned Chinese medicine extraction concentrated solution be Chinese medicine single medicinal material or compound recipe with water or other conventional Extraction solvent, through suitably extracting, the concentrated concentrated solution obtained; Also through variable concentrations precipitate with ethanol, filtration, the concentrated concentrated solution obtained after can be Chinese medicine single medicinal material or compound recipe water extraction.
The solid content of above-mentioned Chinese medicine extraction concentrated solution is at 0%-50%, and relative density (measures under room temperature) between 0 to 2.0.
Above-mentioned composite auxiliary material is the mixture of plasdoneS-630, light magnesium oxide and maltodextrin, plasdoneS-630 consumption accounts for the 0.1%-10% extracting solid content in concentrated solution, light magnesium oxide consumption accounts for the 0.1%-15% extracting solid content in concentrated solution, and maltodextrin consumption accounts for the 0.1%-5% extracting solid content in concentrated solution.
Above-mentioned drying means can be drying under reduced pressure, constant pressure and dry, spraying dry, lyophilization etc.
Beneficial effect of the present invention:
1. the inventive method is simple, and only need add a small amount of composite auxiliary material in extract concentration process, composite auxiliary material dissolubility is good, substantially can not extend the production time.
2. various adjuvants contained in this composite auxiliary material are preparation and commonly use adjuvant, take rear avirulence and untoward reaction.
3. adjuvant addition is few, improves the compliance of patient, cheap, maximizedly reduces production cost.
4. this composite auxiliary material not only can improve the softening point of material, has protection against the tide simultaneously, improves the features such as Chinese medicine preparation raw material mobility, facilitates the preparation of preparation and improves the quality of the pharmaceutical preparations.
(4) accompanying drawing explanation
Fig. 1 is reference substance loganin chromatograms
Fig. 2 is the chromatograms of Fructus Corni extract powder I and Fructus Corni extract powder II
Fig. 3 is the chromatograms of composite auxiliary material
Fig. 4 is the chromatograms of pinoresinol diglucoside
Fig. 5 is the chromatograms of eucommia ulmoides extract powder I and eucommia ulmoides extract powder II
Fig. 6 is the chromatograms of composite auxiliary material
Fig. 7 is the chromatograms of chlorogenic acid
Fig. 8 is the chromatograms of hawthorn extract powder I and hawthorn extract powder II
Fig. 9 is the chromatograms of composite auxiliary material
Figure 10 potenlin Accumulation dissolution
(5) detailed description of the invention
Embodiment 1
The preparation of Fructus Corni extract powder
Get Fructus Corni aqueous extract (ρ=1.035, solid content 0.35%) 250mL, after spraying dry, obtain Fructus Corni extract powder I.
Get Fructus Corni aqueous extract (ρ=1.035, solid content 10%) 250mL, add the dissolving of 10%plasdoneS-630,15% light magnesium oxide and 1% maltodextrin according to accounting for the percentage ratio extracting concentrated solution solid content and mix with Fructus Corni extracting solution, after spraying dry, obtaining Fructus Corni extract powder II.
The mensuration of softening point
Utilize Vicat softening point tester to measure the softening point of Fructus Corni extract powder, experimental result sees the following form:
Table 1 Fructus Corni extract powder softening point measurement result
Experimental result shows, after adding adjuvant, the softening point of Fructus Corni extract powder II significantly improves.
Composite auxiliary material is to the investigation of Fructus Corni effective ingredient disturbed condition
The preparation of reference substance solution: get loganin reference substance 4.0mg, accurately weighed, put in 100mL volumetric flask, with 80% dissolve with methanol and to scale, shake up and get final product.
The preparation of need testing solution: get Fructus Corni extract powder I, each 0.1g of Fructus Corni extract powder II, accurately weighed, put in 25mL volumetric flask, add 80% methanol solution to scale, weighed weight, ultrasonic 30min, is cooled to room temperature, weighed weight again, supply the weight of less loss with 80% methanol, shake up, get supernatant filter membrane (0.45 μm) and filter, get subsequent filtrate, HPLC measures.
The preparation of negative control solution: get composite auxiliary material and prepare negative control solution by need testing solution preparation method.
Get each 10 μ l sample introductions of reference substance solution, need testing solution and negative control solution respectively, record liquid chromatogram.Fig. 1 is reference substance loganin chromatograms, and Fig. 2 is the liquid phase figure of Fructus Corni extract powder I and Fructus Corni extract powder II, Fig. 3 is the chromatograms of composite auxiliary material.
From Fig. 1, Fig. 2, Fig. 3, loganin chromatographic peak peak shape is symmetrical, in test sample chromatogram, loganin peak energy is separated well with other composition, composite auxiliary material does not disturb substantially to other main components in the index composition loganin of Fructus Corni extract powder II and chromatograms, and in the chromatograms of Fructus Corni extract powder I and Fructus Corni extract powder II, main component does not also change substantially.
Embodiment 2
The preparation of eucommia ulmoides extract powder
Get Cortex Eucommiae aqueous extract (ρ=0.994, solid content 0.35%) 250mL, carry out spraying dry, obtain eucommia ulmoides extract powder I.
Get Cortex Eucommiae aqueous extract (ρ=0.994, solid content 0.35%) 250mL, add 7%plasdoneS-630,7% light magnesium oxide and 3% maltodextrin and dissolve, mix with Cortex Eucommiae extracting solution and carry out spraying dry, obtain eucommia ulmoides extract powder II.
The mensuration of softening point
Utilize melting point apparatus to measure the softening point of Cortex Eucommiae traditional Chinese medicinal extract powder, experimental result sees the following form:
Table 2 eucommia ulmoides extract powder softening point measurement result
Experimental result shows, after adding adjuvant, the softening point of eucommia ulmoides extract powder II significantly improves.
Composite auxiliary material is to the investigation of Cortex Eucommiae effective ingredient disturbed condition
The preparation of reference substance solution: it is appropriate that precision takes pinoresinol diglucoside reference substance, adds methanol and makes the solution of every 1mL containing 0.5mg, shake up, to obtain final product.
The preparation of need testing solution: get eucommia ulmoides extract powder I and eucommia ulmoides extract powder II0.1g, accurately weighed, put in apparatus,Soxhlet's, add chloroform appropriate, reflux 6 hours, discards chloroform liquid, put again in apparatus,Soxhlet's, add methanol in right amount, reflux 6 hours, extracting solution reclaims methanol to appropriate, is transferred in 10mL measuring bottle, adds methanol to scale, shake up, filter, get subsequent filtrate, to obtain final product.
The preparation of negative control solution: get composite auxiliary material and prepare negative control solution by need testing solution preparation method.
Get each 10 μ l sample introductions of reference substance solution, need testing solution and composite auxiliary material solution respectively, record liquid chromatogram.Fig. 4 is the chromatograms of pinoresinol diglucoside, and Fig. 5 is the chromatograms of eucommia ulmoides extract powder I and eucommia ulmoides extract powder II, and Fig. 6 is the chromatograms of composite auxiliary material.
Symmetrical from Fig. 4, Fig. 5, Fig. 6 visible pinoresinol diglucoside reference substance chromatographic peak peak shape, in test sample chromatogram, pinoresinol diglucoside peak energy is separated well with other composition, composite auxiliary material does not disturb other main components in the index composition pinoresinol diglucoside of eucommia ulmoides extract powder II and chromatograms, and the main component in eucommia ulmoides extract powder I and eucommia ulmoides extract powder II chromatograms does not change substantially.
Embodiment 3
The preparation of hawthorn extract powder
Get Fructus Crataegi aqueous extract (ρ=1.01, solid content 6.8%) 250mL, carry out spraying dry, obtain hawthorn extract powder I.
Get Fructus Crataegi aqueous extract (ρ=1.01, solid content 6.8%) 250mL, add 3%plasdoneS-630,8% light magnesium oxide and 5% maltodextrin and dissolve, mix with hawthorn extract and carry out spraying dry, obtain hawthorn extract powder II.The mensuration of softening point
Utilize melting point apparatus to measure the softening point of Fructus Crataegi traditional Chinese medicinal extract powder, experimental result sees the following form:
Table 3 eucommia ulmoides extract powder softening point measurement result
Experimental result shows, after adding adjuvant, the softening point of hawthorn extract powder II significantly improves.
Composite auxiliary material is to the investigation of Fructus Crataegi effective ingredient disturbed condition
The preparation of reference substance solution: weigh 3.92mg, be placed in the brown volumetric flask of 10mL, dilutes standardize solution with 50% dissolve with methanol, obtains 392ug/mL mother solution; Dilute 10 times, obtain 39.2ug/mL contrast solution.
The preparation of need testing solution: get hawthorn extract powder I and each 0.1g of hawthorn extract powder II, add 50% methanol constant volume to 25mL volumetric flask, ultrasonic 10min, filters, gets subsequent filtrate, to obtain final product.
The preparation of negative control solution: get composite auxiliary material and prepare negative control solution by need testing solution preparation method.
Get each 10 μ l sample introductions of reference substance solution, need testing solution and negative control solution respectively, record liquid chromatogram.Fig. 7 is the chromatograms of chlorogenic acid, and Fig. 8 is the chromatograms of hawthorn extract powder I and hawthorn extract powder II, and Fig. 9 is the chromatograms of composite auxiliary material.
From Fig. 7, Fig. 8, Fig. 9, visible chlorogenic acid reference substance chromatographic peak peak shape is symmetrical, test sample chromatogram Content of Chlorogenic Acid peak energy is separated well with other composition, composite auxiliary material does not disturb substantially to other the main component in the index composition chlorogenic acid of hawthorn extract powder II and chromatograms, and the main component in hawthorn extract powder I and hawthorn extract powder II chromatograms does not also change substantially.
Embodiment 4
The preparation of potenlin extract powder
Get potenlin extracting solution (after 10 times amount water extraction, 60% ethanol precipitate with ethanol, is concentrated into ρ=1.05 to medical material, solid content 10.7%) 250mL and carry out spraying dry, obtain potenlin extract powder I.
(medical material is after 10 times amount water extraction to get potenlin aqueous extract, 60% ethanol precipitate with ethanol, be concentrated into ρ=1.05, solid content 10.7%) 250mL, 0.1%plasdoneS-630+ adds 5% light magnesium oxide+5% dextrin and dissolves, mixes and carry out spraying dry, obtains potenlin extract powder II.
The mensuration of softening point
Utilize melting point apparatus to measure the softening point of potenlin traditional Chinese medicinal extract powder, experimental result sees the following form:
Table semi-finals power peaceful extract powder softening point measurement result
Experimental result shows, after adding adjuvant, the softening point of potenlin extract powder II significantly improves.
Composite auxiliary material is to the investigation of index composition interference in potenlin prescription
Prepare 0.1mol/L hydrochloric acid solution simulation simulated gastric fluid according to version Chinese Pharmacopoeia in 2005 two annex XD, ultrasonic 15min is degassed.Version Chinese Pharmacopoeia two annex XC the 3rd method small-radius curve track in 2005 is adopted to measure, simulated gastric fluid consumption 250mL, rotating speed 50rpm, temperature (37 ± 5) DEG C, get 0.5 ~ 1.0g spray powder end, respectively 5,15,30,60,90,120min samples 5mL (adding equal-volume equality of temperature simulated gastric fluid after sampling), 0.45 μm of filtering with microporous membrane, get subsequent filtrate, take simulated gastric fluid as blank, HPLC measures, and obtains preparation, and do release rate to curve during the time, as shown in Figure 10.
Result shows: the preparation of extract after 15min, more than 75%, meets release requirement.Illustrate that this composite auxiliary material does not disturb substantially to index composition syringoside in potenlin compound recipe.
Claims (4)
1. improve a method for Chinese medicine preparation raw material softening point, it is characterized in that: in the Chinese medicine extraction concentrated solution that softening point is low, add appropriate composite auxiliary material, stir and make it dispersed, will can obtain the higher extractum powder of softening point after concentrated solution drying; Above-mentioned composite auxiliary material is the mixture of plasdoneS-630, light magnesium oxide and maltodextrin, plasdoneS-630 consumption accounts for the 0.1%-10% extracting solid content in concentrated solution, light magnesium oxide consumption accounts for the 0.1%-15% extracting solid content in concentrated solution, and maltodextrin consumption accounts for the 0.1%-5% extracting solid content in concentrated solution.
2. a kind of method improving Chinese medicine preparation raw material softening point according to claim 1, is characterized in that: pending Chinese medicine extraction concentrated solution be Chinese medicine single medicinal material or compound recipe with water or other conventional Extraction solvent, through suitably extracting, the concentrated concentrated solution obtained; Also through variable concentrations precipitate with ethanol, filtration, the concentrated concentrated solution obtained after can be Chinese medicine single medicinal material or compound recipe water extraction.
3. a kind of method improving Chinese medicine preparation raw material softening point according to claim 1, is characterized in that: the solid content of pending Chinese medicine extraction concentrated solution is at 0%-50%; Relative density is between 0 to 2.0.
4. a kind of method improving Chinese medicine preparation raw material softening point according to claim 1, is characterized in that: above-mentioned drying means is drying under reduced pressure, constant pressure and dry, spraying dry or lyophilization.
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| 现代中药制剂开发中药用新辅料的应用概况;林华庆等;《药品评价》;20060228;第3卷(第1期);第70页左栏倒数第1段 * |
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Effective date of registration: 20191230 Address after: 201203 Shanghai city Pudong New Area Cailun Road No. 1200 Patentee after: Shanghai University of Traditional Chinese Medicine Address before: 201203 Shanghai Cailun Road, room 423 No. 781 Patentee before: Shanghai Zhangjiang Traditional Chinese Medicine Modern Pharmaceutical Preparation Technology Engineering Research Center |