CN104173470B - A kind of preparation method of Colophonium pharmaceutical composition - Google Patents
A kind of preparation method of Colophonium pharmaceutical composition Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of Colophonium pharmaceutical composition, mixing after two taste medical material Herba Pogostemonis in Colophonium pharmaceutical composition and Radix Et Rhizoma Rhei are extracted, again by elite composite resin post and preferred technological parameter, make general anthraquinone and total flavones obtain maximum enriching and purifying simultaneously, take into account yield and purity, simplification of flowsheet, resource of saving time.In the anthraquinone flavone mixture that optimum process of the present invention is obtained, total anthraquinones content is more than 35%, and yield is more than 50%, and general flavone content is more than 45%, and total flavones yield is more than 50%.
Description
Technical field
The present invention relates to a kind of preparation method of Chinese medicine composition, particularly a kind of preparation method of Colophonium pharmaceutical composition, belongs to medical art.
Background technology
Colophonium granule records in national drug standards part, standard number: WS-10902 (ZD-0902)-2002, and prescription is as follows: Radix Et Rhizoma Rhei 200g, Herba Pogostemonis 200g, sucrose 800g, makes 1000g.Its traditional preparation methods is: above two taste medical materials, and Radix Et Rhizoma Rhei powder is broken into coarse powder, adds alcohol reflux secondary, each 1.5 hours, filters; Herba Pogostemonis extraction by steam distillation volatile oil, aqueous solution filters, and filtrate and Radix Et Rhizoma Rhei extract merge, and are concentrated into the clear paste that relative density is 1.30 ~ 1.35 (50 DEG C), add cane sugar powder, make granule, dry, let cool, spray adds above-mentioned volatile oil, and mixing, to obtain final product.The method is not extracted Herba Pogostemonis flavone.
According to document, the main composition of Radix Et Rhizoma Rhei is general anthraquinone, and the main composition of Herba Pogostemonis is volatile oil and total flavones, therefore for the medicine containing these two kinds of medical materials, conventional way first extracts, then adopt macroporous resin or polyamide to refine respectively targetedly.But carry out respectively by medical material for the refining concentrated of two kinds of compositions under normal circumstances, namely obtain general anthraquinone and total flavones respectively, complex operation, production cycle are long.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of Colophonium pharmaceutical composition.By the purification step of general anthraquinone and total flavones is merged and the optimization of technological parameter, reach simplification of flowsheet and take into account the object of yield and purity.
Technical solution of the present invention is as follows:
A preparation method for Colophonium pharmaceutical composition, comprises the steps:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200 weight portion, extracts with steam distillation and collects volatile oil, and adopts beta-schardinger dextrin-to carry out enclose to volatile oil in conventional manner, obtains volatile oil clathrate compound;
(2) preparation of general anthraquinone and total flavones concentrated solution: step (1) Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.15-1.25, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200 weight portion are extracted respectively, respectively add ethanol extraction 2-3 time of percent by volume 60-80%, the amount of alcohol of the 60-80% added is the 6-10 times amount volume of medical material weight, extraction time 1-2h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and total flavones concentrated solution respectively;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions step (2) obtained merge, get supernatant to mix with the clear distillate that step (2) obtains, the sample concentration being configured to medical material that adds water is that every 2-4ml solution is containing 1g medical material, applied sample amount is 4-6BV, loading flow velocity is 1-2BV/h, refining resin is that AB-8 macroporous resin mixes by 2:1 ~ 1:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 70-80% ethanol for eluant, eluant volume is 4-5BV, elution flow rate 1-2BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture,
(4) mix: get the obtained anthraquinone flavone mixture 15-25 weight portion mix homogeneously of the obtained volatile oil clathrate compound 15-21 weight portion of step (1), step (3) and get final product.
The present invention is preferred, a kind of preparation method of Colophonium pharmaceutical composition, and in the preparation of wherein step (3) anthraquinone flavone mixture, resin used is that AB-8 macroporous resin mixes with polyamide the composite resin formed by 1.5:1 weight ratio.
The present invention is preferred, a kind of preparation method of Colophonium pharmaceutical composition, in the preparation of wherein step (3) anthraquinone flavone mixture, sample concentration is that every 4ml solution is containing 1g medical material, applied sample amount is 4BV, loading flow velocity is 2BV/h, first uses the water elution of 3BV after composite resin post adsorbs, flow velocity 2BV/h, discard water lotion, again with percent by volume 70% ethanol for eluant, eluant volume is 4BV, elution flow rate 1BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture.
The present invention is preferred further, a kind of preparation method of Colophonium pharmaceutical composition, in the preparation of wherein step (2) general anthraquinone and total flavones concentrated solution, concentration of alcohol used is 70%, extraction time is 3 times, 70% ethanol contend added is respectively 10,8,8 compared to the multiple of two kinds of medical material formulation weight, and extraction time is respectively 2h, 1h and 1h.
The present invention is preferred again, a kind of preparation method of Colophonium pharmaceutical composition, wherein the preparation method of step (1) volatile oil clathrate compound is: get Herba Pogostemonis 200 parts by weight, adds the water of medical material gross weight 8 times amount volume, adopts steam distillation to extract and collects volatile oil; Volatile oil is dissolved in equivalent dehydrated alcohol, add in the beta-schardinger dextrin-aqueous solution of percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, keep temperature 50 C, stir 3h, 0-4 DEG C of refrigerated overnight, sucking filtration, must precipitate, 50 DEG C of vacuum dryings, obtain volatile oil clathrate compound.
The present invention is also preferred, a kind of preparation method of Colophonium pharmaceutical composition, and wherein in step (4) mixing, the weight ratio of volatile oil clathrate compound and anthraquinone flavone mixture is 18:20.
The unit of above weight portion and parts by volume is grams per milliliter.
Beneficial effect of the present invention is as follows:
Mixing after two taste medical material Herba Pogostemonis in Colophonium pharmaceutical composition prescription and Radix Et Rhizoma Rhei extract by the present invention, again by elite composite resin post and preferred technological parameter, make general anthraquinone and total flavones obtain maximum enriching and purifying simultaneously, take into account yield and purity, simplification of flowsheet, resource of saving time.In the anthraquinone flavone mixture that wherein optimum process is obtained, total anthraquinones content is more than 35%, and yield is more than 50%, and general flavone content is more than 45%, and total flavones yield is more than 50%.Compare the independent enriching and purifying of total flavones and general anthraquinone, products therefrom yield is suitable with purity, but the step that greatly simplifies the operation.
Term explanation
Concentration of alcohol of the present invention is percent by volume; BV is column volume or claims bed volume.
Accompanying drawing explanation
Fig. 1 is the impact of different proportion hybrid resin on yield;
Fig. 2 is the impact of different proportion hybrid resin on purity;
Fig. 3 is the impact of different sample concentration on adsorption rate;
Fig. 4 is the impact of different applied sample amount on adsorption rate;
Fig. 5 is that different loading flow velocity is on the impact of adsorption rate;
Fig. 6 is the impact of different eluant strength on desorption efficiency;
Fig. 7 is that different eluant volume is on the impact of desorption efficiency;
Fig. 8 is the impact of different elution flow rate on desorption efficiency;
Wherein, the vertical coordinate of the vertical coordinate of Fig. 1 to be the vertical coordinate of yield (%), Fig. 2 be purity (%), Fig. 3-Fig. 8 is adsorption rate (%), and in abscissa, Fig. 1, Fig. 2 are AB-8: the weight ratio of polyamide; Fig. 3 is sample concentration (ml medicinal liquid/g medical material); Fig. 4 is applied sample amount (BV); Fig. 5 is loading flow velocity (BV/h); Fig. 6 is eluant strength (percent by volume %); Fig. 7 is eluant volume (BV); Fig. 8 is elution flow rate (BV/h).
Detailed description of the invention
In order to illustrate in greater detail the present invention, provide following specific experiment example and embodiment.But scope of the present invention is not limited thereto.Being that raw material of the present invention is not done to illustrate is commercially available.
Experimental example 1, inclusion essential oil technological experiment
The present invention is studied inclusion essential oil technique, with volatile oil envelop rate, clathrate yield for index, the factors such as beta-schardinger dextrin-consumption, amount of water, enclose temperature, enclose time are investigated, result shows the beta-schardinger dextrin-aqueous solution selecting percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, and 3 hours enclose time, when enclose temperature is 50 DEG C, clathrate yield and inclusion essential oil rate, more than 90%, can satisfy the demands.
The polishing purification technological experiment of experimental example 2, anthraquinone flavone mixture
1. instrument and reagent
UV-2450 type Shimadzu ultraviolet spectrophotometer; KQ5200B type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.); Shimadzu AUW220D electronic balance.Chromatography polyamide (30-60 order, rub fast science equipment company limited in Shanghai); LSA-21, XDA-8, D101 macroporous resin (Xi'an Lanxiao Sci-Tech Co., Ltd., medical grade); AB-8, ADS-17, HPD-300, NKA-9 macroporous resin (Cangzhou Bao En Chemical Co., Ltd., medical grade).Herba Pogostemonis, rhubarb medicinal material is all purchased from Guangdong Da Rentang prepared slices of Chinese crude drugs company limited (Herba Pogostemonis lot number: 20131211, Radix Et Rhizoma Rhei lot number: 20131205).All the other reagent etc. are analytical pure.
2. method and result
2.1 general anthraquinone concentrated solutions preparations: get the ethanol extraction three times that rhubarb medicinal material 200g adds percent by volume 70%, first time adds 2000ml, extract 2 hours, second and third time respectively adds 1600ml, each extraction 1 hour, merge extractive liquid, decompression recycling ethanol is extremely without alcohol taste, centrifugal, supernatant water is configured to 4 times amount volumes of medical material gross weight, obtains general anthraquinone concentrated solution 800ml;
2.2 total flavones concentrated solution preparations: get Herba Pogostemonis medical material 200g, extraction by steam distillation volatile oil, Aqueous extracts filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.15-1.25, adds ethanol furnishing percent by volume 70% determining alcohol, and 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains precipitate with ethanol concentrated solution for subsequent use; Medicinal residues add the ethanol extraction three times of percent by volume 70%, and first time adds 10 times amount of medical material gross weight, and extracts 2 hours, second and third time respectively adds 8 times amount of medical material gross weight, all extracts 1 hour, merge extractive liquid, decompression recycling ethanol, extremely without alcohol taste; Merge above-mentioned precipitate with ethanol concentrated solution and alcohol extraction concentrated solution, centrifugal, supernatant water is configured to 4 times amount volumes of medical material gross weight, obtains total flavones concentrated solution 800ml.
The purity testing of 2.3 general anthraquinones and total flavones
2.3.1 general anthraquinone standard curve preparation: get emodin reference substance 5.0mg, accurately weighed, put in 25ml volumetric flask, add dissolve with methanol and be settled to scale, shaking up, to obtain final product.Precision measure reference substance solution 0.5,1.0,1.5,2.0,2.5,3.0ml, put in 25ml measuring bottle respectively, add 1% magnesium acetate methanol solution and be diluted to scale, shake up, place, colour developing 30min, absorbance is measured respectively at 509nm place, with emodin reference substance concentration (μ g/ml) for abscissa, absorbance is vertical coordinate, obtained standard curve A=0.00181C+0.00334 (r=0.9997).
2.3.2 sample general anthraquinone purity testing: sample thief dried cream powder 0.5g, accurately weighed, put in 10ml volumetric flask, add methanol appropriate, supersound process 30min, is placed to room temperature, adds methanol constant volume to scale, shakes up, as need testing solution.Precision measures above-mentioned need testing solution 1ml, puts in 25ml volumetric flask, adds 1% magnesium acetate methanol solution and is diluted to scale, shake up, and places, and colour developing 30min, measures absorbance A respectively at 509nm place, calculated purity, computing formula
2.3.3 total flavones standard curve preparation: get control substance of Rutin 10mg, accurately weighed, put in 50ml measuring bottle, add 70% appropriate amount of ethanol, ultrasonic dissolution, let cool, add 70% ethanol to scale, shake up, obtain (every 1ml is containing rutin 0.2mg).Precision measures reference substance solution 1ml, 2ml, 3ml, 4ml, 5ml, 6ml, put in 25ml measuring bottle respectively, respectively add water to 6.0ml, add 5% sodium nitrite solution 1ml, mixing, place 6 minutes, add 10% aluminum nitrate solution 1ml again, shake up, place 6 minutes, hydro-oxidation sodium test solution 10ml, add water to scale again, shake up, place 15 minutes, take corresponding reagent as blank, according to ultraviolet visible spectrophotometry (annex VA), absorbance is measured at the wavelength place of 500nm (or 510nm), take absorbance as vertical coordinate, concentration is abscissa, obtained standard curve A=0.00057C-0.01522 (r=0.9998).
2.3.4 sample total flavones purity testing: sample thief dried cream powder 0.5g, puts in 10ml volumetric flask, accurately weighed, 70% appropriate amount of ethanol, and ultrasonic dissolution, lets cool, and adds 70% ethanol to scale, shakes up, as need testing solution.Precision measures need testing solution 1ml, puts in 25ml measuring bottle, and the method under sighting target directrix curve preparation, from " adding water to 6ml ", measures absorbance A, calculated purity, computing formula in accordance with the law
The screening of 2.4 macroporous resins: 1. static adsorption: precise 8 kinds of each 20g of resin, often kind of resin takes two parts, add two kinds of each 40ml of concentrated solution (every 4ml medicinal liquid is equivalent to 1g medical material) respectively, put jolting 24h on shaking table, filter, measure the absorbance of filtrate, calculate the adsorption rate of each resin according to standard curve Equation for Calculating general anthraquinone and total flavones concentration.2. steady-state solution absorption: the resin after sucking filtration, adds 85% ethanol 50ml desorption, be placed on shaking table, after 8h, filter, measure the absorbance of filtrate, calculates each resin desorption rate according to standard curve Equation for Calculating general anthraquinone and total flavones concentration.3. purity testing: the desorbing attached liquid of filtration, drying under reduced pressure gets dry extract powder, carries out mensuration and calculated purity according to " purity testing of 2.3 general anthraquinones and total flavones " method.
Yield (%)=adsorption rate (%) × desorption efficiency (%)
Result shows, and in yield % and purity %, in 8 kinds of resins, AB-8 resin is best to total Radix Et Rhizoma Rhei anthraquinone concentration effect, and polyamide is best to Herba Pogostemonis total flavones concentration effect.The results are shown in Table 1, table 2.
Table 1 different model resin is to the comparison of Absorption of Anthraquinones in Radix Et performance
| Resin model | Adsorption rate (%) | Desorption efficiency (%) | Yield (%) | Purity (%) |
| Polyamide | 63.29 | 76.46 | 48.39 | 33.58 |
| LSA-21 | 61.42 | 75.89 | 46.61 | 30.67 |
| XDA-8 | 69.17 | 65.25 | 45.13 | 28.74 |
| D101 | 64.32 | 72.51 | 46.64 | 35.65 |
| AB-8 | 65.37 | 75.86 | 49.59 | 37.28 |
| ADS-17 | 58.93 | 77.27 | 45.54 | 31.74 |
| HPD-300 | 66.25 | 73.43 | 48.65 | 29.47 4 --> |
| NKA-9 | 60.34 | 72.87 | 43.97 | 27.46 |
Table 2 different model resin is to the comparison of Herba Pogostemonis total flavones absorption property
| Resin model | Adsorption rate (%) | Desorption efficiency (%) | Yield (%) | Purity (%) |
| Polyamide | 61.32 | 81.34 | 49.88 | 48.07 |
| LSA-21 | 60.31 | 81.15 | 48.94 | 42.31 |
| XDA-8 | 73.39 | 60.85 | 44.66 | 39.64 |
| D101 | 72.59 | 67.24 | 48.81 | 41.57 |
| AB-8 | 67.45 | 71.54 | 48.25 | 43.34 |
| ADS-17 | 59.86 | 71.94 | 43.06 | 46.07. |
| HPD-300 | 65.72 | 75.01 | 49.30 | 40.15 |
| NKA-9 | 56.03 | 81.27 | 45.54 | 44.21 |
2.5 mixed with resin ratios screenings: in order to simplification of flowsheet, after the extraction concentrated solution of Radix Et Rhizoma Rhei and Herba Pogostemonis merges by this experiment, by the composite resin post of AB-8 resin and polyamide mixing, the optimum mixture ratio filtering out two kinds of resins is routine.Method, with the screening of 2.4 macroporous resins, the results are shown in Table 3, Fig. 1, Fig. 2.
The comparison of table 3 different proportion hybrid resin absorption property
As can be seen from table 3 and Fig. 1, Fig. 2, AB-8 and polyamide two kinds of resins mix according to different proportion, all impact is had on the yield of total Radix Et Rhizoma Rhei anthraquinone and Herba Pogostemonis total flavones and purity, wherein the yield of general anthraquinone slowly declines along with the raising of AB-8 ratio in hybrid resin, the yield of total flavones then increases gradually along with the raising of AB-8 ratio in hybrid resin, the AB-8 that two intersections of complex curve of yield are corresponding: the ratio of polyamide is about 1.5:1, and now total flavones and the yield both general anthraquinone are about 51%; In purity curve, the ratio of two kinds of resins is 1 ~ 2 time, and purity slows down, and is substantially in plateau even no longer to change after especially ratio is greater than 2, and the now purity of total flavones about 45%, the purity of general anthraquinone is about 37%.Therefore, consider, select 2:1 ~ 1:1 ratio better, now both yields all can reach more than 50%, and especially the ratio of 1.5:1 is best, and according to curve, both yields all can reach 51%, and purity is also higher.
2.6 hybrid resin absorption property checkings:
Get total Radix Et Rhizoma Rhei anthraquinone concentrated solution respectively, the each 80ml of mixed concentrated liquid (every 4ml medicinal liquid is equivalent to 1g medical material) of Herba Pogostemonis total flavones concentrated solution and the two 1:1, each via hybrid resin post, (AB-8 resin and polyamide 1.5:1 mix, 40g), and respectively with the concentration of 4ml medicinal liquid/g medical material, the amount of liquid medicine of 4 times of BV, by hybrid resin post, (AB-8 resin and polyamide 1.5:1 mix the flow velocity of 2BV/h, 20g) adsorb, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, use 70% ethanol elution of 4BV again, elution flow rate 1BV/h, collect eluent respectively, and calculate corresponding adsorption rate and desorption efficiency, the desorbing attached liquid filtered, drying under reduced pressure gets dry extract powder, carries out purity testing according to " assay of 2.3 general anthraquinones and total flavones " method.
Yield (%)=adsorption rate (%) × desorption efficiency (%)
The absorption property checking of table 4 hybrid resin
Result: in table 4, result shows, and in yield % and purity %, hybrid resin separates enrichment and mix concentration effect similar to total Radix Et Rhizoma Rhei anthraquinone, Herba Pogostemonis total flavones, and yield and purity reach expected results.
The screening of 2.7 resin purification techniques: in view of the impact of elution parameters on purity is less, for convenience of experiment, on the above results basis, this experiment continues with the adsorption rate of general anthraquinone and total flavones and desorption efficiency for index, investigates affecting the loading parameter (sample solution concentration, applied sample amount, loading flow velocity) of purifying process and elution parameters (eluant strength, eluant volume, elution flow rate) etc.
2.7.1 the investigation of sample concentration: the extraction concentrated solution of Radix Et Rhizoma Rhei and Herba Pogostemonis is merged, be configured to 2 respectively, 4,6, the concentration loading of 8ml medicinal liquid/g medical material, calculate the adsorption rate of total flavones and general anthraquinone, the results are shown in Table 5, Fig. 3.Result shows, at identical flow velocity with under identical adsorption time, adsorption rate and sample concentration are inversely proportional to, more favourable to absorption at low concentrations, but concentration is too low, medicine liquid volume amount is too large, loading cycle stretch-out, therefore comprehensive two aspects are considered to determine best upper 4ml medicinal liquid/g medical material, and namely loading medicine liquid volume number is equivalent to 4 times of medical material gross weight.
2.7.2 the investigation of applied sample amount: respectively with the amount of liquid medicine loading of 3,4,5,6 times of column volumes (BV), calculates the adsorption rate of total flavones and general anthraquinone, the results are shown in Table 5, Fig. 4.Result shows, and the absorption of resin to total flavones and general anthraquinone is directly proportional to applied sample amount substantially, and when 4 times of column volumes, adsorption curve is mild gradually, and absorption is tending towards saturated, and therefore best loading volume is 4BV.
2.7.3 the investigation of loading flow velocity: respectively with 1,2,3,4,5, the flow velocity of 6BV/h by resin column, calculate the adsorption rate of total flavones and general anthraquinone, the results are shown in Table 5, Fig. 5.Result shows, and along with the raising of loading flow velocity, the adsorption rate of total flavones and general anthraquinone constantly reduces, and 1BV/h and 2BV/h effect is more or less the same, and therefore considers from time saving angle, determines using 2BV/h as best loading flow velocity.
2.7.4 the investigation of eluant strength: after medicinal liquid is adsorbed by resin column, after 3BV distillation washing post, respectively by volume parts than the ethanol elution being 30%, 50%, 70%, 85%, 4BV collected by often kind of eluent, and calculating desorption efficiency, the results are shown in Table 6, Fig. 6.As can be seen from the results, along with the continuous increase of concentration of alcohol, desorption efficiency constantly rises, when after arrival 70%, desorption efficiency increases not obvious, and namely concentration of alcohol increases the desorbing impact of flavone little again, therefore consider from the angle of conservation, choose the optium concentration that 70% is eluant.
2.7.5 the investigation of elution volume: after medicinal liquid is adsorbed by resin column, after 3BV distillation washing post, then carry out eluting with the flow velocity of 1BV/h respectively with 70% ethanol, 1BV collects portion, calculates the desorption efficiency of total flavones and general anthraquinone, the results are shown in Table 6, Fig. 7.Found that, when eluent is 4BV, substantially reach desorbing balance, now increase effluent volume more little on desorption efficiency impact, therefore selected 4BV is as preferred elution volume.
2.7.6 the investigation of elution flow rate: after medicinal liquid is adsorbed by resin column, after 3BV distillation washing post, then with 70% ethanol respectively with 1,2,3, the flow velocity of 4BV/h carries out eluting, calculating total flavones and general anthraquinone desorption efficiency, the results are shown in Table 6, Fig. 8.Result shows, elution flow rate is faster, and desorption efficiency is less, and during 1BV/h, desorption efficiency is maximum, therefore determines with 1BV/h for best elution flow rate.
The different loading parameter of table 5 is on the impact of adsorption rate
Seen by the result of table 5 and Fig. 3-5, with the concentration of 4ml medicinal liquid/g medical material, the amount of liquid medicine loading of 4 times of BV, the flow velocity of 2BV/h is adsorbed by composite resin post, and effect is better.
The different elution parameters of table 6 is on the impact of desorption efficiency
3, conclusion
By above experimental result, finally determine that resin purification technique is: with the amount of liquid medicine loading of the concentration of 4ml medicinal liquid/g medical material, 4 times of BV, the flow velocity of 2BV/h is adsorbed by composite resin post, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, then use 70% ethanol elution of 4BV, elution flow rate 1BV/h.
Following examples for understanding the present invention, but are not limited thereto.
The preparation method of embodiment 1, a kind of Colophonium pharmaceutical composition, comprising:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200g, extract with steam distillation and collect volatile oil, beta-schardinger dextrin-is adopted to carry out enclose to volatile oil, beta-schardinger dextrin-aqueous solution percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, and 3 hours enclose time, when enclose temperature is 50 DEG C, obtain volatile oil clathrate compound 18.5g, yield 92.1%; ;
(2) preparation of general anthraquinone and total flavones concentrated solution: above-mentioned Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.20, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200g extract respectively, respectively add the ethanol extraction 3 times of percent by volume 70%, the amount of alcohol added respectively is respectively 2000ml, 1600ml and 1600ml, extraction time is respectively 2h, 1h and 1h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and each 150ml of total flavones concentrated solution respectively;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions merge, get supernatant to mix with clear distillate, the sample concentration being configured to medical material that adds water is that every 4ml solution is containing 1g medical material, applied sample amount is 4BV, loading flow velocity is 2BV/h, refining resin is that AB-8 macroporous resin mixes by 1.5:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 70% ethanol for eluant, eluant volume is 4BV, elution flow rate 1BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture 20.8g, wherein general anthraquinone yield 52.1%, purity 36.9%, total flavones yield 51.3%, purity 47.4%,
(4) mix: get volatile oil clathrate compound 18g, anthraquinone flavone mixture 20g mix homogeneously and get final product.
The preparation method of embodiment 2, a kind of Colophonium pharmaceutical composition, comprising:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200g, extract with steam distillation and collect volatile oil, beta-schardinger dextrin-is adopted to carry out enclose to volatile oil, beta-schardinger dextrin-aqueous solution percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, and 3 hours enclose time, when enclose temperature is 50 DEG C, obtain volatile oil clathrate compound 17.1g, yield 90.8%;
(2) preparation of general anthraquinone and total flavones concentrated solution: above-mentioned Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.15, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200g extract respectively, respectively add the ethanol extraction 2 times of percent by volume 60%, the amount of alcohol added is 1200ml, extraction time is 1h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and each 150ml of total flavones concentrated solution respectively;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions merge, get supernatant to mix with clear distillate, the sample concentration being configured to medical material that adds water is that every 2ml solution is containing 1g medical material, applied sample amount is 4BV, loading flow velocity is 1BV/h, refining resin is that AB-8 macroporous resin mixes by 2:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 70% ethanol for eluant, eluant volume is 4BV, elution flow rate 1BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture 18.4g, wherein general anthraquinone yield 46.6%, purity 37.1%, total flavones yield 46.1%, purity 47.2%,
(4) mix: get volatile oil clathrate compound 15g, anthraquinone flavone mixture 18g mix homogeneously and get final product.
The preparation method of embodiment 3, a kind of Colophonium pharmaceutical composition, comprising:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200g, extract with steam distillation and collect volatile oil, beta-schardinger dextrin-is adopted to carry out enclose to volatile oil, beta-schardinger dextrin-aqueous solution percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, and 3 hours enclose time, when enclose temperature is 50 DEG C, obtain volatile oil clathrate compound 19.3g, yield 93.0%;
(2) preparation of general anthraquinone and total flavones concentrated solution: above-mentioned Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.25, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200g extract respectively, respectively add the ethanol extraction 3 times of percent by volume 80%, the amount of alcohol added is 2000ml respectively, extraction time is 2h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and each 150ml of total flavones concentrated solution respectively; ;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions merge, get supernatant to mix with clear distillate, the sample concentration being configured to medical material that adds water is that every 3ml solution is containing 1g medical material, applied sample amount is 5BV, loading flow velocity is 2BV/h, refining resin is that AB-8 macroporous resin mixes by 1:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 80% ethanol for eluant, eluant volume is 5BV, elution flow rate 2BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture 22.6g, wherein general anthraquinone yield 51.5%, purity 34.2%, total flavones yield 50.1%, purity 44.3%,
(4) mix: get volatile oil clathrate compound 18g, anthraquinone flavone mixture 21g mix homogeneously and get final product.
The preparation method of embodiment 4, a kind of Colophonium pharmaceutical composition, comprising:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200g, extract with steam distillation and collect volatile oil, beta-schardinger dextrin-is adopted to carry out enclose to volatile oil, beta-schardinger dextrin-aqueous solution percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, and 3 hours enclose time, when enclose temperature is 50 DEG C, obtain volatile oil clathrate compound 18.2g, yield 91.7%;
(2) preparation of general anthraquinone and total flavones concentrated solution: above-mentioned Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.15-1.25, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200g extract respectively, respectively add the ethanol extraction 2 times of percent by volume 70%, the amount of alcohol added is 1600ml, extraction time is respectively 2h, 1h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and each 150ml of total flavones concentrated solution respectively;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions merge, get supernatant to mix with clear distillate, the sample concentration being configured to medical material that adds water is that every 4ml solution is containing 1g medical material, applied sample amount is 6BV, loading flow velocity is 1BV/h, refining resin is that AB-8 macroporous resin mixes by 1.5:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 80% ethanol for eluant, eluant volume is 4BV, elution flow rate 1BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture 19.3g, wherein general anthraquinone yield 48.8%, purity 35.4%, total flavones yield 47.2%, purity 46.5%,
(4) mix: get volatile oil clathrate compound 18g, anthraquinone flavone mixture 18g mix homogeneously and get final product.
Claims (6)
1. a preparation method for Colophonium pharmaceutical composition, is characterised in that, comprises the steps:
(1) preparation of volatile oil clathrate compound: get Herba Pogostemonis 200 weight portion, extracts with steam distillation and collects volatile oil, and adopts beta-schardinger dextrin-to carry out enclose to volatile oil in conventional manner, obtains volatile oil clathrate compound;
(2) preparation of general anthraquinone and total flavones concentrated solution: step (1) Herba Pogostemonis extracts the Aqueous extracts after volatile oil and filters, being evaporated to relative density at 50 DEG C is the clear paste of 1.15-1.25, add ethanol furnishing percent by volume 70% concentration of alcohol, 2-10 DEG C leaves standstill 24 hours, filter, decompression filtrate recycling ethanol, to without alcohol taste, obtains distillate clearly, stand-by; Herba Pogostemonis medicinal residues after extraction volatile oil, Radix Et Rhizoma Rhei 200 weight portion are extracted respectively, respectively add ethanol extraction 2-3 time of percent by volume 60-80%, the amount of alcohol of the 60-80% added is the 6-10 times amount volume of medical material weight, extraction time 1-2h, merge extractive liquid, decompression recycling ethanol, to without alcohol taste, obtains general anthraquinone concentrated solution and total flavones concentrated solution respectively;
(3) preparation of anthraquinone flavone mixture: centrifugal after two kinds of concentrated solutions step (2) obtained merge, get supernatant to mix with the clear distillate that step (2) obtains, the sample concentration being mixed with medical material that adds water is that every 2-4ml solution is containing 1g medical material, applied sample amount is 4-6BV, loading flow velocity is 1-2BV/h, refining resin is that AB-8 macroporous resin mixes by 2:1 ~ 1:1 the composite resin post formed with polyamide and adsorbs, the water elution of 3BV is first used after absorption, flow velocity 2BV/h, discard water lotion, again with 70-80% ethanol for eluant, eluant volume is 4-5BV, elution flow rate 1-2BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture,
(4) mix: get the obtained anthraquinone flavone mixture 15-25 weight portion mix homogeneously of the obtained volatile oil clathrate compound 15-21 weight portion of step (1), step (3) and get final product.
2. the preparation method of a kind of Colophonium pharmaceutical composition according to claim 1, be characterised in that, in the preparation of step (3) anthraquinone flavone mixture, resin used is that AB-8 macroporous resin mixes with polyamide the composite resin formed by 1.5:1 weight ratio.
3. the preparation method of a kind of Colophonium pharmaceutical composition according to claim 1, be characterised in that, in the preparation of wherein step (3) anthraquinone flavone mixture, sample concentration is that every 4ml solution is containing 1g medical material, applied sample amount is 4BV, loading flow velocity is 2BV/h, first uses the water elution of 3BV after composite resin post adsorbs, flow velocity 2BV/h, discard water lotion, again with percent by volume 70% ethanol for eluant, eluant volume is 4BV, elution flow rate 1BV/h, collect eluent, concentrating under reduced pressure, dry, obtain anthraquinone flavone mixture.
4. the preparation method of a kind of Colophonium pharmaceutical composition according to claim 1, be characterised in that, concentration of alcohol used in the preparation of step (2) general anthraquinone and total flavones concentrated solution is 70%, extraction time is 3 times, 70% ethanol contend added is respectively 10,8,8 compared to the multiple of two kinds of medical material formulation weight, and extraction time is respectively 2h, 1h and 1h.
5. the preparation method of a kind of Colophonium pharmaceutical composition according to claim 1, be characterised in that, the preparation method of step (1) volatile oil clathrate compound is: get Herba Pogostemonis 200 parts by weight, add the water of medical material gross weight 8 times amount volume, adopt steam distillation to extract and collect volatile oil; Volatile oil is dissolved in equivalent dehydrated alcohol, add in the beta-schardinger dextrin-aqueous solution of percent weight in volume 6%, the envelope-bulk to weight ratio of volatile oil and beta-schardinger dextrin-is 1ml:6g, keep temperature 50 C, stir 3h, 0-4 DEG C of refrigerated overnight, sucking filtration, must precipitate, 50 DEG C of vacuum dryings, obtain volatile oil clathrate compound.
6. the preparation method of a kind of Colophonium pharmaceutical composition according to claim 1, is characterised in that, in step (4) mixing, the weight ratio of volatile oil clathrate compound and anthraquinone flavone mixture is 18:20.
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