CN102114155A - Serial Chinese medicinal preparation for treating phaseolus cold and preparation process and quality control method thereof - Google Patents
Serial Chinese medicinal preparation for treating phaseolus cold and preparation process and quality control method thereof Download PDFInfo
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Abstract
The invention discloses a serial Chinese medicinal preparation for treating phaseolus cold, a preparation process and a quality control method thereof. Preparations are characterized by being prepared from traditional Chinese medicines, namely platycodon root, tangerine peel, indigowoad leaf, weeping forsythiae, nutgrass galingale rhizome, perilla leaf, fineleaf schizonepeta herb, divaricate saposhnikovia root and liquoric root as well as pharmaceutical excipients. The preparation has the effects of clearing away heat and relieving exterior syndromes, and is used for symptoms such as fever and headache, running nose, cough and dry mouth and the like caused by phaseolus cold. Volatile oil is a material base of clearing away heat and relieving exterior syndromes of the preparation; and the traditional preparation process is to adopt a way of spraying the volatile oil into the preparation, and the volatile oil is almost completely lost during the production and storage due to the low content of the volatile oil, so that the clinical therapeutic effect is seriously affected. In the preparation process, a volatile oil inclusion process is adopted, so the loss of the volatile oil during the production and storage is reduced, and the stability of a medicine is improved and the clinical therapeutic effect of the medicine is ensured at the same time. In addition, the more perfect quality control method is used for ensuring the quality; meanwhile, the clinical medication formulation is also enriched, so that the clinical medication demand can be better met.
Description
Technical field
The invention belongs to field of traditional Chinese, relate to a kind of serial Chinese medicine preparation and preparation technology and method of quality control for the treatment of four seasons common cold.
Background technology
Flu is commonly called as " cold ", is also referred to as upper respiratory tract infection, is a kind of respiratory tract commonly encountered diseases that is caused by multiple virus, and onset is more anxious, and early symptom has pharyngeal dried itching or burning sensation, sneeze, nasal obstruction, watery nasal discharge, can be with pharyngalgia.Chinese medicine thinks that flu is because ailment said due to cold or exposure when taking advantage of human body to drive evil scarce capacity, and the invasion and attack lung is defended due to the fur.See so that wind and cold, two kinds of syndromes of wind heat more clinically." four seasons common cold sheet " records in the 13 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, and its prescription is: Radix Platycodonis 167g, Folium Perillae 250g, Pericarpium Citri Reticulatae 167g, Herba Schizonepetae 125g, Folium Isatidis 167g, Fructus Forsythiae 167g, Radix Glycyrrhizae (processing) 83g, Rhizoma Cyperi (stir-fry) 167g, Radix Saposhnikoviae 125g; Method for making is: above nine flavors are broken into fine powder with balloonflower powder; Folium Perillae, Pericarpium Citri Reticulatae, Herba Schizonepetae are extracted volatile oil to most, the aqueous solution after the distillation, and device is collected in addition; Folium Isatidis, Fructus Forsythiae, Radix Glycyrrhizae decoct with water secondary, and each 2 hours, collecting decoction filtered, and the aqueous solution after filtrate and the above-mentioned distillation merges, and being condensed into relative density is the clear paste of 1.32～1.36 (60～65 ℃ of surveys); Rhizoma Cyperi, Radix Saposhnikoviae were with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, merge extractive liquid, filters, and filtrate is regained ethanol to there not being the alcohol flavor, and be condensed into the clear paste that relative density is 1.32～1.36 (60～65 ℃ of surveys), with above-mentioned clear paste and Radix Platycodonis fine powder mixing, drying, pulverize, granulate, spray into volatile oil with dissolve with ethanol, mixing airtight 2 hours, is pressed into 1000, sugar coating, promptly.Its reasonable recipe specially at anemofrigid cold, is selected the Chinese medicine of clearing away heat and expelling pathogen in the exterior such as Folium Perillae, Herba Schizonepetae, Pericarpium Citri Reticulatae for use, is used for the fever and headache that four seasons anemofrigid cold causes, rhinorrhea with clear discharge, and the cough xerostomia is had sore throat, the anorexia of feeling sick.Its property of medicine is gentle, and curative effect is safe, is applicable to all kinds of flu crowds, and old, anemia of pregnant woman and child are particularly suitable.Remarkable in view of its clinical efficacy, therefore have multiplely on the basis of tablet at present, carry out the kind of form improvement, as capsule, granule, pill etc.
Modern chemistry composition and pharmacological research show, volatile oil component is the main matter basis of clearing away heat and expelling pathogen in the exterior class medicines such as Folium Perillae, Herba Schizonepetae, Pericarpium Citri Reticulatae, therefore, in the preparation technology of four seasons common cold sheet, the extraction of volatile oil is very crucial, and it effectively extracts, and reasonably adds, rational preparation process, each step is all to guaranteeing that curative effect all has appreciable impact.The preparation process of the four seasons common cold sheet of stipulating in the primary standard is to be to be sprayed in the granule in last preparation process with volatile oil, carries out tabletting.The enterprise of domestic production four seasons common cold sheet reaches tens of families at present, also still continues to use the technology that traditional volatile oil sprays.We are carrying out in the research process this kind, find: (1) in process of production, volatile oil is sprayed in the process of technological operations such as granule and oven drying at low temperature, packing, elegant volatilization, volatile oil component loses up to more than 20%; (2) finished product through test determination, is placed the tablet of half a year in depositing process, and its volatile oil component has lost more than 50%; (3) in addition, the continuous effusion of volatile oil has not only influenced curative effect, and also the stability to product has produced destruction (for example bellding, pit etc. appear in the sheet sub-surface).Above-mentioned situation has all had a strong impact on the clinical efficacy of this product.
In addition, Chinese patent 200410045023.0 discloses a kind of four seasons common cold capsule and preparation method thereof, and it is only reformed on dosage form, but the volatile oil that adopts also is to spray, and also has the deficiency that curative effect can not fine performance; Chinese patent 200810081948.9 discloses a kind of four seasons common cold pill, be to reform by the four seasons common cold tablet form, though its volatile oil adopts cyclic dextrin clathrate, but this dosage form pill is compared with tablet and capsule, exist onset slower, the characteristics that bioavailability is lower, the patient considers dosage forms such as rapid-action tablet, capsule, granule usually on dosage form selection.
Summary of the invention
The purpose of this invention is to provide a kind of serial Chinese medicine preparation for the treatment of four seasons common cold.Specifically be meant four seasons common cold sheet, four seasons common cold capsule and four seasons common cold granule.They have overcome the weak point of preparation technology aspect the main effective ingredient volatile oil content of assurance of former four seasons common cold sheet, adopt beta-schardinger dextrin-inclusion technology, volatile oil in the prescription is carried out inclusion, can effectively reduce the loss of finished product volatile oil in processes such as production and storage, and make finished product more stable.
Another object of the present invention is on the basis perfect to preparation technology, carry out rational form improvement, develop disintegrate is faster, bioavailability is higher capsule and granule,, adapt to the requirement of vast flu patient different dosage form for this prescription has increased novel form again.
Another purpose of the present invention is to be optimized on extraction process and to screen, and optimizes amount of water, alcohol adding amount, makes process conditions clearer and more definite.
A further object of the present invention is to adopt different auxiliary material to screen in the capsule formulation process, preferably is beneficial to the adjuvant of capsule molding, has guaranteed the stability of finished product.Wherein said adjuvant comprises filler and lubricant, and wherein filler is selected from a kind of of starch, dextrin, lactose or two kinds or three kinds, and its consumption is 15%～35%; Lubricant is selected from a kind of of magnesium stearate, sodium lauryl sulphate or two kinds, and its consumption is 0.6%～1.2%.
A further object of the present invention is to adopt different auxiliary material to screen in the granular preparation process, preferably is beneficial to the adjuvant of granule molding, has guaranteed the stability of finished product.Wherein said adjuvant is selected from a kind of of dextrin, lactose or two kinds, and its consumption is 15%～50%.
A further object of the present invention is that preparation has been carried out detailed deep quality standard research, improves on the basis of primary standard.Under the 13 four seasons common cold sheet item that records of former " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, only the thin layer of rationalization discriminating and Radix Platycodonis is differentiated, this product is in development process, the medical material of respectively distinguishing the flavor of in the prescription has all been carried out more deep Study on Identification, improve the thin layer discrimination method of Radix Platycodonis, set up Herba Schizonepetae, Fructus Forsythiae, Radix Glycyrrhizae, Rhizoma Cyperi, the thin layer discriminating of Radix Saposhnikoviae and the content assaying method of phillyrin.Can control the quality of this product effectively, guarantee clinical efficacy.
Technical scheme of the present invention is: with Radix Platycodonis 167 weight portions, be ground into fine powder; Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions extract volatile oil to the greatest extent, obtain volatile oil or volatile oil distillate, the aqueous solution after the distillation, and device is collected in addition; Volatile oil or volatile oil distillate stir inclusion with beta-schardinger dextrin-and become inclusion complex; Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae (processing) 83 weight portions decoct with water secondary, each 2 hours, collecting decoction, filter, the aqueous solution merging after filtrate and the above-mentioned distillation, being condensed into and recording relative density at 60～65 ℃ is 1.32～1.36 clear paste; Rhizoma Cyperi (stir-fry) 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, merge extractive liquid, filtered, filtrate is regained ethanol to there not being the alcohol flavor, and is condensed into that to record relative density at 60～65 ℃ be 1.32～1.36 clear paste; With above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, be extraction extractum of the present invention.
Extract in the extractum in the present invention, add 10%～25% starch, 2%～5% microcrystalline Cellulose, 0.5%～1.0% magnesium stearate, mixing, tabletting is tablet of the present invention.
Extract in the extractum in the present invention, add a kind of of 15%～35% starch, dextrin, lactose or two kinds or three kinds, 0.6%～1.2% magnesium stearate, sodium lauryl sulphate a kind of or two kinds incapsulate, and are capsule of the present invention.
Extract extractum in the present invention, add a kind of of 15%～50% dextrin, lactose or two kinds, mixing, granulate is made granule, and pack is granule of the present invention.
Using method of the present invention: oral, one time 3～5, or 3～5, or 1～2 bag, 3 times on the one.
The invention has the beneficial effects as follows:
(1) volatile oil to Folium Perillae, Pericarpium Citri Reticulatae, Herba Schizonepetae in the prescription carries out inclusion, and volatile oil be these series of products material bases of onset rapidly in clinical practice, and the way that traditional handicraft adopts volatile oil to spray into is in production with to deposit in the process loss of volatile oil serious.After adopting beta-schardinger dextrin-inclusion technology, reduce loss of volatile oil in production and the storage, guaranteed curative effect of medication; With the liquid drug solidification, improved stability of drug.
(2) carried out improving and raising of quality standard.Under the 13 four seasons common cold sheet item that records of former " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, only the thin layer of rationalization discriminating and Radix Platycodonis is differentiated, this product is in development process, the medical material of respectively distinguishing the flavor of in the prescription has all been carried out more deep Study on Identification, improve the thin layer discrimination method of Radix Platycodonis, set up Herba Schizonepetae, Fructus Forsythiae, Radix Glycyrrhizae, Rhizoma Cyperi, the thin layer discriminating of Radix Saposhnikoviae and the content assaying method of phillyrin.Can control the quality of this product more effectively, guarantee clinical efficacy.
(3) capsule of the present invention and granule are the kinds of carrying out form improvement on the basis of former four seasons common cold sheet tablet, compare with tablet, capsule and the granule disintegrate is faster, bioavailability is higher, increased two novel forms again for this prescription simultaneously, can fully adapt to the requirement of vast flu patient different dosage form.
Below the adjuvant of volatile oil inclusion technology in foregoing invention tablet, capsule and the granular preparation process and capsule further screened and optimize by test.
Test 1: the selection of inclusion equipment
Though at present domestic have the document of many inclusion essential oil technology to deliver, but its content is confined to the research of laboratory lab scale substantially, really inclusion essential oil technology and equipment are successfully applied to the actually rare of the big production of Chinese medicine, and do not have the special equipment of volatile oil inclusion on the present state giving drugs into nose machine equipment market.We design jointly with equipment producer, have customized special beta-cyclodextrin inclusion compound equipment according to production technology characteristic.This production technology is in a retort, and (having independently steam-heated pipe line, can satisfied temperature be 30 ℃-60 ℃ inclusion reaction condition can to finish enclose continuously; Has double-deck stirring paddle, can guarantee volatile oil and β-abundant mixing of CD solution, react completely), Cryoprecipitation (has the brine ice cooling pipe simultaneously, can satisfy the condition of 0-10 ℃ of Cryoprecipitation 24h) and filter separation (lower end is furnished with filter, and supernatant is once emitted, fluid of inclusion complex suspension) process, the operation and the number of turnover have been reduced, an equipment batch can reach 100kg, and is easy and simple to handle, the production efficiency height.
Test 2: volatile oil distillate inclusion process conditions are preferred
With orthogonal table L9 (3
4) optimum process condition of screening Folium Perillae, Pericarpium Citri Reticulatae, Herba Schizonepetae volatile oil distillate β-CD anti-package knot, the factor level table sees Table 1.
Table 1 factor level table
Inclusion method: the distillate 100ml that gets known volatile oil content, get 9 parts altogether, in relevant temperature (60 ℃, 50 ℃, 40 ℃), constant temperature, under 300 rev/mins of stirrings of rotating speed, add β-CD (4g, 3g, 2g), and continuing to stir inclusion to stipulated time (4h, 3h, 2h), refrigerator and cooled is hidden 24h, filters, the cold water washing inclusion complex, drain the back in 50 ℃ of dryings, weigh, calculate the inclusion complex recovery rate.
Inclusion the results are shown in Table 2 and table 3:
Table 2 L9 (3
4) orthogonal table
Table 3 analysis of variance table
F
1-0.1(2，2)＝9 F
1-0.05(2，2)＝19 F
1-0.01(2，2)＝99
Result of the test shows that every 100ml distillate adds β-CD addition 4.0g, and whipping temp is 40 ℃, and mixing time is 3h, and volatile oil inclusion rate is higher.
Test 3: volatile oil inclusion process conditions are preferred
Use orthogonal table L
9(3
4) having screened the optimum process condition of inclusion essential oil, the factor level table sees Table 4.
Table 4 factor level table
2.2.2 inclusion method: get β-CD solution (6g → 150ml), get 9 parts altogether, under relevant temperature (40 ℃, 50 ℃, 60 ℃) constant temperature, under 300 rev/mins of stirrings of rotating speed, add volatile oil (1.5ml, 1.0ml, 0.75ml), and continue to stir enclose to stipulated time (2,3,4h), refrigerator and cooled is hidden 24h, filter, the cold water washing clathrate is drained the back in 60 ℃ of dryings, weigh, calculate the clathrate recovery rate.
Weight method records volatile oil density: 0.817g/ml
Testing program and the results are shown in Table 5, variance analysis sees Table 6.
Table 5 L
9(3
4) orthogonal table
Table 6 analysis of variance table
F
1-0.1(2，2)＝9 F
1-0.05(2，2)＝19 F
1-0.01(2，2)＝99
Result of the test shows, is 1ml: 6g with oil: β-CD, mixing time 3h, and temperature is that 40 ℃ clathrate process is better.
Test 4: relatively the different adding modes of volatile oil are to the influence of volatile oil content
(1) respectively with the four seasons common cold capsule (technology one: the volatile oil beta cyclodextrin clathrate adds, technology two: volatile oil sprays and adds) of different process preparation, measures according to Chinese Pharmacopoeia version appendix in 2005 X D determination of volatile oil method (first method).
Test method: get each 1000 of test samples respectively, get content, porphyrize, enable pass is crossed sieve No. three, and mix homogeneously, respectively taking technique one, each 200g of technology two samples (oil content is about 1.2ml), get two parts respectively, divide another name to decide weight (accurately to 0.01g), put in the 1000ml flask, add water 500ml and zeolite, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube, put in the electric jacket, extract volatile oil to most, about 5 hours, put coldly, read the volatile oil volume, the results are shown in Table 7.
The four seasons common cold capsule volatile oil content of table 7 different process preparation relatively
Result of the test shows: according to the sample of technology one (adding of volatile oil beta cyclodextrin clathrate) preparation, in preparation process, the volatile oil content loss only is 11.7%, according to the sample of technology two (volatile oil sprays and adds) preparation, in preparation process, volatile oil content is with a toll of more than 20%.
(2) sample of the sample of taking technique one and technology two, room temperature was placed after 6 months, carried out volatile oil content relatively, by above-mentioned determination of volatile oil experimental condition operation, the results are shown in Table 8:
The four seasons common cold capsule volatile oil content of table 8 different process preparation relatively
(room temperature was placed after 6 months)
Result of the test shows: the four seasons common cold capsule volatile oil content according to technology one (adding of volatile oil betacyclodextrin clathrate) preparation is not seen loss in depositing process, and has lost nearly 50% according to the four seasons common cold capsule volatile oil of technology two (volatile oil sprays and adds) preparation.
The above results shows, adopts the four seasons common cold capsule of volatile oil betacyclodextrin inclusion prepared, and volatile oil is in preparation and put procedure, and loss is few, can more effective assurance clinical efficacy.
Below by test the adjuvant in the above-mentioned granular preparation process is further screened and optimizes.
Test 5: the granulate investigation of used dextrin, lactose addition of four seasons common cold granule
In granular preparation technology, dextrin, the different additions of lactose and particle appearance, the uniformity, hygroscopicity, melting are investigated.Select suitable preparation process through testing sieve, now screening study be summarized as follows:
(1) qinghuo reagent 740g adds balloonflower powder 160g, adds lactose 450g mixing, granulation gained granule, and color distortion is bigger, and melting is good, easily moisture absorption, it is the moisture absorption caking that the granule room temperature is placed 20 minutes, packed products moisture absorption in 30 days is hardened.
(2) qinghuo reagent 740g adds balloonflower powder 160g, adds dextrin 150g, lactose 300g mixing, granulation gained granule, and outward appearance is even, and melting is good, and the granule room temperature is placed 24 hours no changes, packed products no significant change in 6 months.
(3) qinghuo reagent 740g adds balloonflower powder 160g, adds dextrin 270g, lactose 180g mixing, granulation gained granule, and outward appearance is even, and melting is good, and the granule room temperature is placed 24 hours no changes, packed products no significant change in 6 months.
(4) qinghuo reagent 740g adds balloonflower powder 160g, adds dextrin 450g mixing, granulation gained granule, and outward appearance is even, and melting is good, and the granule room temperature is placed 24 hours no changes, packed products no significant change in 6 months.
Table 9 preparation process catalog
According to result of the test,, comparatively suitable with technology (2)～(4) through many batches of scale-ups.
Test 6: the one-step palletizing conditional filtering reaches with wet granulation and compares
Marumerization: mealiness adjuvants such as the dextrin in will writing out a prescription, lactose powder drop in the truck of one-step-granulating method, and setting temperature of charge is 60～80 ℃, and the blower fan frequency is 25～45Hz.Rise and to close the granulation chamber, start blower fan, make air by air-vent through just, medium effeciency filter, enter the granulation chamber by container bottom again, material is fluctuated mixes and preheating.Open the atomizing pressure switch, the adjustment atomizing pressure is 0.1～0.3MPa.Start peristaltic pump, the adjustment flow velocity is 6～20Hz, and the fluid extract that sprays in the prescription is granulated.In this process, adjust relevant technological parameter at any time, and check the granule character, till qualified from observation panel.After cooling was shut down, discharging got final product.
Wet granulation: mealiness adjuvants such as the dextrin in will writing out a prescription, lactose powder drop in the wet granulator, start the stirring at low speed slurry with mixing of materials 15min, add the Chinese medicine fluid extract of recipe quantity, granulate with the high-speed stirred cutting.Through 70 ℃ of dryings 6～8 hours, granulate promptly.
Adopt the four seasons common cold granule of two kinds of method preparations all to meet the pharmacopeia requirement, but quality is variant slightly, the results are shown in Table 10,11.
The four seasons common cold granular mass of 2 kinds of method preparations of table 10 is estimated
Table 11 preparation technology evaluation
Experimental result shows that this product adopts conventional wet to granulate when producing, and need pass through each road production operation such as mixing, granulation, granulate, drying successively, total preparation time is longer, and multiple working procedure needs material to shift, and not only material loss is higher, working strength is also bigger, needs to be equipped with more personnel.The particle size distribution uniformity of this method preparation is general, and yield is lower, and particle properties differs greatly between batch.
The granule of marumerization preparation, operations such as its mixing, granulation, drying can be finished in an equipment simultaneously, and preparation time is short, and material loss is few, and working strength is lower, only needs to be equipped with a small amount of personnel.The technological operation and the parameter of one-step palletizing are more stable, good reproducibility, and made particle surface and loose and porous inner surface, bulk density is little, and dissolution rate is fast, and is better mobile, epigranular, the yield height is so adopt marumerization to prepare this product granule.
Test 7: capsule formulation is screened with adjuvant
1. the starch addition determines
Consider Chinese medicinal capsule agent easy moisture absorption in put procedure, therefore add into adjuvant, investigate, need to add the starch of medicated powder weight 10%～14%, see Table 12 through several batches of finished products than tablet.
Starch addition in each batch sample of table 12
2. the investigation of magnesium stearate addition
Other gets the granule that makes, and adds magnesium stearate in 0.4%, 0.7%, 1.0% ratio respectively, and mixing the results are shown in Table 13.
The investigation of table 13 magnesium stearate addition
The magnesium stearate addition is 0.7～1.0% o'clock, and mobile good fluidity is easy to encapsulated.
Test 8: tablet formulation adjuvant screening
1. the consumption of magnesium stearate is investigated
Get the granule that makes, add magnesium stearate in 0.4%, 0.7%, 1.0% ratio respectively, other adds 5% microcrystalline Cellulose, mixing, and tabletting the results are shown in Table 14 respectively.
Table 14 magnesium stearate addition is to the influence of tablet weight variation
The magnesium stearate addition is 0.4% o'clock, and tablet weight variation is bigger, and 2 overruns are arranged; When the magnesium stearate addition is 0.5%-1.0%, label smooth surface, smooth, no sliver phenomenon.
2. the consumption of microcrystalline Cellulose is investigated
Because the corner is easy to wear during the tablet coating that is pressed into, and is easy to break, thus consider to add microcrystalline Cellulose improving particulate cohesive and compressibility, and the microcrystalline Cellulose consumption has been done investigation.
Get the granule that makes, add microcrystalline Cellulose in 2%, 4%, 5% ratio respectively, other adds 1% magnesium stearate, mixing, and tabletting the results are shown in Table 15 respectively.
Table 15 microcrystalline Cellulose addition is to the influence of label
According to result of the test, select for use 2～5% microcrystalline Cellulose good as the label quality that adjuvant makes, be beneficial to coating, and few to the heavy increment of sheet.
Below by specific embodiment particulate extraction formulation method of four seasons common cold sheet, four seasons common cold capsule and four seasons common cold and method of quality control are described in further detail.
Embodiment
Embodiment 1:
With Radix Platycodonis 167 weight portions, be ground into fine powder; Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions add 12 times of water gagings and extract volatile oil 3 hours to the greatest extent, the aqueous solution after the distillation, and device is collected in addition; (100ml: 1g) stir 2h at 40 ℃, inclusion becomes inclusion complex to the volatile oil distillate with beta-schardinger dextrin-; Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae 83 weight portions, decoct with water secondary, each 2 hours, amount of water is respectively 12 times, 10 times, collecting decoction, filter, the aqueous solution after filtrate and the above-mentioned distillation merges, and being condensed into relative density is the clear paste of 1.32～1.36 (60～65 ℃ of surveys); Rhizoma Cyperi 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, alcohol adding amount is respectively 12 times, 10 times, and merge extractive liquid, filters, filtrate is regained ethanol to there not being the alcohol flavor, and is condensed into that to record relative density at 60～65 ℃ be 1.32～1.36 clear paste; With above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, drying is pulverized, and granulates, and promptly gets preparation granules.
Embodiment 2:
With Radix Platycodonis 167 weight portions, be ground into fine powder; Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions add 12 times of water gagings and extract volatile oil 4 hours to the greatest extent, the aqueous solution after the distillation, and device is collected in addition; (100ml: 6g) stir 4h at 60 ℃, inclusion becomes inclusion complex to the volatile oil distillate with beta-schardinger dextrin-; Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae 83 weight portions, decoct with water secondary, each 2 hours, amount of water is respectively 12 times, 10 times, collecting decoction, filter, the aqueous solution after filtrate and the above-mentioned distillation merges, and being condensed into relative density is the clear paste of 1.32～1.36 (60～65 ℃ of surveys); Rhizoma Cyperi 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, alcohol adding amount is respectively 12 times, 10 times, and merge extractive liquid, filters, filtrate is regained ethanol to there not being the alcohol flavor, and is condensed into that to record relative density at 60～65 ℃ be 1.32～1.36 clear paste; With above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, drying is pulverized, and granulates, and promptly gets preparation granules.
Embodiment 3:
With Radix Platycodonis 167 weight portions, be ground into fine powder; Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions add 12 times of water gagings and extract volatile oil 4 hours to the greatest extent, the aqueous solution after the distillation, and device is collected in addition; Get volatile oil, (0.3g: 100ml), stir 4h at 60 ℃, inclusion becomes inclusion complex in the adding beta-schardinger dextrin-aqueous solution (4%); Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae 83 weight portions, decoct with water secondary, each 2 hours, amount of water is respectively 12 times, 8 times, collecting decoction, filter, the aqueous solution after filtrate and the above-mentioned distillation merges, and being condensed into relative density is the clear paste of 1.32～1.36 (60～65 ℃ of surveys); Rhizoma Cyperi 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, alcohol adding amount is respectively 12 times, 8 times, and merge extractive liquid, filters, filtrate is regained ethanol and is not distinguished the flavor of to there being alcohol, and is condensed into the clear paste that relative density is 1.32～1.36 (60～65 ℃ of surveys); With above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, drying is pulverized, and granulates, and promptly gets preparation granules.
Embodiment 4:
With Radix Platycodonis 167 weight portions, be ground into fine powder; Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions add 8 times of water gagings and extract volatile oil 3 hours to the greatest extent, the aqueous solution after the distillation, and device is collected in addition; Get volatile oil, (1.1g: 100ml), stir 2h at 40 ℃, inclusion becomes inclusion complex in the adding beta-schardinger dextrin-aqueous solution (4%); Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae 83 weight portions, decoct with water secondary, each 2 hours, amount of water is respectively 12 times, 8 times, collecting decoction, filter, the aqueous solution after filtrate and the above-mentioned distillation merges, and being condensed into relative density is the clear paste of 1.32～1.36 (60～65 ℃ of surveys); Rhizoma Cyperi 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, alcohol adding amount is respectively 12 times, 8 times, and merge extractive liquid, filters, filtrate is regained ethanol and is not distinguished the flavor of to there being alcohol, and is condensed into the clear paste that relative density is 1.32～1.36 (60～65 ℃ of surveys); With above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, drying is pulverized, and granulates, and promptly gets preparation granules.
Embodiment 5:
To add 60g starch in any extraction dried particles in the various embodiments described above, the 15g microcrystalline Cellulose, mixing sieves, and adds the 1.5g magnesium stearate, mixing, tabletting is tablet of the present invention.
Embodiment 6:
To add the 90g lactose in any extraction dried particles in the various embodiments described above, mixing sieves, and adds the 8g magnesium stearate, and mixing incapsulates, and is capsule of the present invention.
Embodiment 7:
To add the 80g dextrin in any extraction dried particles in the various embodiments described above, mixing sieves, and adds the 6g sodium lauryl sulphate, and mixing incapsulates, and is capsule of the present invention.
Embodiment 8:
To add the 250g dextrin in any extraction dried particles in the various embodiments described above, mixing sieves, and uses the aluminum-plastic composite membrane packing, is granule of the present invention.
Embodiment 9:
In the quality control of the present invention, the medical material of respectively distinguishing the flavor of in the prescription is all carried out more deep Study on Identification, improved the thin layer discrimination method of Radix Platycodonis, set up Herba Schizonepetae, Fructus Forsythiae, Radix Glycyrrhizae, Rhizoma Cyperi, the thin layer discriminating of Radix Saposhnikoviae and the content assaying method of phillyrin.
The thin layer of Radix Platycodonis is differentiated as follows: get this product content 2g, add 2% sulfuric acid solution 30ml, reflux 1 hour is put cold, filter, filtrate adds 10% sodium hydroxide solution adjust pH to 5, extracts 2 times with the ether jolting, each 30ml, merge ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Platycodonis control medicinal material 1.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 3 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-glacial acetic acid (3: 2: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The thin layer of Pericarpium Citri Reticulatae, Herba Schizonepetae is differentiated as follows: get this product content 2.5g, add methanol 50ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, puts cold, extract 3 times with water saturated ethyl acetate jolting, each 15ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Pericarpium Citri Reticulatae control medicinal material 1g, adds methanol 20ml, and reflux 30 minutes is put coldly, filters, and gets subsequent filtrate as Pericarpium Citri Reticulatae control medicinal material solution; Get Herba Schizonepetae control medicinal material 2g again, add methanol 40ml, reflux 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as Herba Schizonepetae control medicinal material solution.Get the Hesperidin reference substance again, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 3 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-methanol-water (50: 7: 4) is developing solvent, launches, and takes out, dry, spray is with 1% aluminum chloride alcoholic solution, and hot blast drying is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, respectively with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The thin layer of Fructus Forsythiae is differentiated as follows: get Fructus Forsythiae control medicinal material 2g, add methanol 30ml, supersound process 30 minutes filters, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 3 times with the chloroform jolting, each 15ml, merge chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Other gets the phillyrin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw [assay] item need testing solution 5 μ l, control medicinal material solution 3 μ l and reference substance solution 3 μ l down, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-glacial acetic acid (70: 8: 3) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
The thin layer of Radix Glycyrrhizae is differentiated as follows: get this product content 2g, add methanol 30ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 3 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid extracts 3 times with 2% sodium carbonate test solution jolting, each 25ml merges alkali liquor, adds hydrochloric acid adjust pH to 1～2, extract 3 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.5g in addition, the 50ml that adds diethyl ether, reflux 30 minutes, ether solution discards, and medicinal residues volatilize, and remainingly shine medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with ethyl acetate-glacial acetic acid-methanol-water (15: 1: 1: 2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The thin layer of Rhizoma Cyperi is differentiated as follows: get this product content 2.5g, add methanol 20ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, puts cold, extract 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Rhizoma Cyperi control medicinal material 2g, adds methanol 40ml, and reflux 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, remainingly shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica GF254 lamellae, with toluene-ethyl acetate-glacial acetic acid (90: 5: 5) is developing solvent, launch, take out, cold wind dries up, and puts under the ultra-violet lamp (254nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
The thin layer of Radix Saposhnikoviae is differentiated as follows: get this product content 4g, add strong ammonia solution 2ml and chloroform 20ml, reflux 1 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Saposhnikoviae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate (7: 3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
In the quality control of the present invention, set up the assay of phillyrin:
Get this product content under the content uniformity item, porphyrize is got about 1.6g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 25ml, evaporate to dryness, residue add hot water 20ml makes dissolving, puts cold, extract 4 times with the chloroform jolting, each 15ml merges chloroform liquid, water 20ml washing, discard water liquid, chloroform liquid evaporate to dryness, residue add ethanol-chloroform (3: 1) mixed liquor 5ml makes dissolving, be added on neutral alumina post (100～200 orders, 1g is on the internal diameter 1～1.5cm), with ethanol 70ml eluting, collect eluent, reclaim ethanol to doing, residue adds ethanol-chloroform (1: 1) mixed liquor makes dissolving, quantitatively is transferred in the 1ml measuring bottle, and add ethanol-chloroform (1: 1) mixed liquor and be diluted to scale, as need testing solution.It is an amount of that other gets the phillyrin reference substance, and accurate the title decides, and adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), accurate need testing solution 8 μ l～10 μ l, reference substance solution 2 μ l and the 4 μ l that draw, putting respectively on same silica gel G precoated plate, is developing solvent with chloroform-methanol-glacial acetic acid (70: 8: 3), launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to develop the color to speckle in about 1～3 minute in 105 ℃ of heating, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side.(an appendix VI of Chinese Pharmacopoeia version in 2005 B) scans wavelength according to thin layer chromatography: λ S=540nm, λ R=700nm measures test sample absorbance integrated value and reference substance absorbance integrated value, calculates, promptly.
Claims (9)
1. serial Chinese medicine preparation for the treatment of four seasons common cold, it is characterized in that its preparation technology is: (1) is ground into fine powder with Radix Platycodonis 167 weight portions; (2) Folium Perillae 250 weight portions, Pericarpium Citri Reticulatae 167 weight portions, Herba Schizonepetae 125 weight portions extract volatile oil to the greatest extent, obtain volatile oil or volatile oil distillate, the aqueous solution after the distillation, and device is collected in addition; (3) volatile oil or volatile oil distillate become inclusion complex with beta-schardinger dextrin-stirring inclusion; (4) Folium Isatidis 167 weight portions, Fructus Forsythiae 167 weight portions, Radix Glycyrrhizae (processing) 83 weight portions decoct with water secondary, each 2 hours, collecting decoction, filter, the aqueous solution merging after filtrate and the above-mentioned distillation, being condensed into and recording relative density at 60～65 ℃ is 1.32～1.36 clear paste; (5) Rhizoma Cyperi (stir-fry) 167 weight portions, Radix Saposhnikoviae 125 weight portions, with 60% ethanol extraction secondary, 2 hours for the first time, 1.5 hours for the second time, merge extractive liquid, filtered, filtrate is regained ethanol to there not being the alcohol flavor, and is condensed into that to record relative density at 60～65 ℃ be 1.32～1.36 clear paste; (6) with above-mentioned clear paste and Radix Platycodonis fine powder mixing, add the volatile oil inclusion complex, promptly get and extract extractum,, granulate as filler with starch, as disintegrating agent, magnesium stearate is as lubricant with microcrystalline Cellulose, and tabletting promptly gets the four seasons common cold sheet.
2. a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1, it is characterized in that extraction extractum in its step of preparation process (6) adds is selected from a kind of of starch, dextrin, lactose or two kinds or three kinds as filler, granulate, be selected from a kind of of magnesium stearate, sodium lauryl sulphate or two kinds as lubricant, incapsulate, promptly get the four seasons common cold capsule.
3. a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1 is characterized in that extraction extractum in its step of preparation process (6) adds to be selected from a kind of of dextrin, lactose or two kinds, mixing, and granulate promptly gets the four seasons common cold granule.
4. a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1 is characterized in that it is 3～6 hours that the described Folium Perillae of its step of preparation process (2), Pericarpium Citri Reticulatae, Herba Schizonepetae are extracted volatile oil to the most time.
5. a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1, it is characterized in that the described volatile oil of its step of preparation process (3) stirs inclusion with beta-schardinger dextrin-and becomes inclusion complex, the ratio of volatile oil and beta-schardinger dextrin-is a weight ratio 0.3～1.1 during inclusion: 4.
6. a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1, it is characterized in that the described volatile oil distillate of its step of preparation process (3) stirs inclusion with beta-schardinger dextrin-and becomes inclusion complex, the ratio of distillate and beta-schardinger dextrin-is volume and weight ratio 100: 1～6 during inclusion.
7. as claim 5,6 described inclusion technologies, it is characterized in that the inclusion temperature is 40 ℃～60 ℃.
8. as claim 5,6 described inclusion technologies, it is characterized in that the inclusion mixing time is 2h～4h.
9. the quality determining method of a kind of serial Chinese medicine preparation for the treatment of four seasons common cold as claimed in claim 1 is as follows:
The thin layer of Radix Platycodonis is differentiated as follows: get this product 2g, add 2% sulfuric acid solution 30ml, reflux 1 hour is put cold, filter, filtrate adds 10% sodium hydroxide solution adjust pH to 5, extracts 2 times with the ether jolting, each 30ml, merge ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Platycodonis control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw need testing solution 3 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with ratio is that normal hexane-ethyl acetate-glacial acetic acid of 3: 2: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The thin layer of Pericarpium Citri Reticulatae, Herba Schizonepetae is differentiated as follows: get this product 2.5g, add methanol 50ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, puts cold, extract 3 times with water saturated ethyl acetate jolting, each 15ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution; Other gets Pericarpium Citri Reticulatae control medicinal material 1g, adds methanol 20ml, and reflux 30 minutes is put coldly, filters, and gets subsequent filtrate as Pericarpium Citri Reticulatae control medicinal material solution; Get Herba Schizonepetae control medicinal material 2g again, add methanol 40ml, reflux 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as Herba Schizonepetae control medicinal material solution; Get the Hesperidin reference substance again, add methanol and make the solution that every 1ml contains 0.4mg, in contrast product solution.Test according to thin layer chromatography, draw each 3 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is that ethyl acetate-methanol-water of 50: 7: 4 is developing solvent, launches, and takes out, dry, spray is with 1% aluminum chloride alcoholic solution, and hot blast drying is put under the ultra-violet lamp of 365nm and inspected; In the test sample chromatograph, respectively with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
The thin layer of Fructus Forsythiae is differentiated as follows: get this product 0.8g, put in the tool plug conical flask, add methanol 50ml, supersound process 30 minutes filters the filtrate evaporate to dryness, residue adds hot water 20ml makes dissolving, puts coldly, extracts 4 times with the chloroform jolting, each 15ml, merge chloroform liquid, water 20ml washing discards water liquid, chloroform liquid evaporate to dryness, it is that ethanol-chloroform mixed liquor 5ml of 3: 1 makes dissolving, is added on 100～200 orders, 1g that residue adds ratio, on the neutral alumina post of internal diameter 1～1.5cm, with ethanol 70ml eluting, collect eluent, reclaim ethanol to doing, it is that ethanol-chloroform mixed liquor 1ml of 1: 1 makes dissolving that residue adds ratio, as need testing solution; Get Fructus Forsythiae control medicinal material 2g, add methanol 30ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 3 times with the chloroform jolting, each 15ml, merge chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution; Other gets the phillyrin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 5 μ l, control medicinal material solution 3 μ l and reference substance solution 3 μ l, put respectively on same silica gel g thin-layer plate, with ratio is that chloroform-methanol-glacial acetic acid of 70: 8: 3 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color;
The thin layer of Radix Glycyrrhizae is differentiated as follows: get this product 2g, add methanol 30ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 3 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid extracts 3 times with 2% sodium carbonate test solution jolting, each 25ml merges alkali liquor, adds hydrochloric acid adjust pH to 1～2, extract 3 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.5g in addition, the 50ml that adds diethyl ether, reflux 30 minutes, ether solution discards, and medicinal residues volatilize, and remainingly shine medical material solution in pairs with legal system; Test according to thin layer chromatography, draw need testing solution 8 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with ratio is 15: 1: 1: ethyl acetate-glacial acetic acid of 2-methanol-water is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
The thin layer of Rhizoma Cyperi is differentiated as follows: get this product 2.5g, add methanol 20ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, puts cold, extract 3 times with the ether jolting, each 20ml merges ether solution, volatilizes, residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Rhizoma Cyperi control medicinal material 2g, adds methanol 40ml, and reflux 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add hot water 15ml makes dissolving, remainingly shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica GF254 lamellae, with ratio is that toluene-ethyl acetate-glacial acetic acid of 90: 5: 5 is developing solvent, launches, and takes out, cold wind dries up, and puts under the ultra-violet lamp of 254nm and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
The thin layer of Radix Saposhnikoviae is differentiated as follows: get this product 4g, add strong ammonia solution 2ml and chloroform 20ml, reflux 1 hour filters, and filtrate evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution; Other gets Radix Saposhnikoviae control medicinal material 1g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be that 60～90 ℃ of petroleum ether-ethyl acetates of boiling range of 7: 3 are developing solvent with ratio, launch, take out, dry, put under the ultra-violet lamp of 365nm and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
The content assaying method of phillyrin is as follows:
Get this product, porphyrize is got about 1.6g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 25ml, evaporate to dryness, residue add hot water 20ml makes dissolving, puts cold, extract 4 times with the chloroform jolting, each 15ml merges chloroform liquid, water 20ml washing discards water liquid, chloroform liquid evaporate to dryness, it is that ethanol-chloroform mixed liquor 5ml of 3: 1 makes dissolving, is added on 100～200 orders, 1g that residue adds ratio, on the neutral alumina post of internal diameter 1～1.5cm,, collect eluent with ethanol 70ml eluting, reclaim ethanol to doing, it is that ethanol-chloroform mixed liquor of 1: 1 makes dissolving that residue adds ratio, quantitatively is transferred in the 1ml measuring bottle, and be diluted to scale, as need testing solution; It is an amount of that other gets the phillyrin reference substance, and accurate the title decides, and adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, accurate need testing solution 8 μ l～10 μ l, reference substance solution 2 μ l and the 4 μ l that draw, putting respectively on same silica gel G precoated plate, is that chloroform-methanol-glacial acetic acid of 70: 8: 3 is developing solvent with ratio, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to develop the color to speckle in about 1～3 minute in 105 ℃ of heating, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side.Scan wavelength according to thin layer chromatography: λ S=540nm, λ R=700nm measures test sample absorbance integrated value and reference substance absorbance integrated value, calculates, promptly.
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