CN101274037A - Composition for curing skin pruritus and preparation method thereof and quality control method - Google Patents
Composition for curing skin pruritus and preparation method thereof and quality control method Download PDFInfo
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Abstract
The invention discloses a pharmaceutical composition for treating skin pruritus, a preparation method and a quality control method thereof. The pharmaceutical composition of the invention consists of crude drugs as follows: fruit of Siberian cocklebur, puncture vine fruit, rhizoma ligustici wallichii, peach kernel and herb of bittersweet. The preparation method is characterized in that: water is added for decoction for 2 to 3 times and 1 to 3 hours for each time, decoction solution is mixed and kept standing for 7 to 9 hours for sedimentation, and supernatant fluid is taken and condensed into clear paste, the relative density of which is 1.36 (65 to 75 DEG C); one portion of the clear paste is taken, three portions of cane sugar powder, one portion of dextrin and a proper amount of ethanol are added to prepare granules which are dried and the pharmaceutical composition is prepared. High performance liquid chromatography is used for determining the content of forulic acid by the invention. The pharmaceutical composition of the invention has very good curing effect for skin pruritus.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, particularly relate to a kind of Chinese medicine composition for the treatment of skin pruritus and preparation method thereof and method of quality control.
Background technology
Skin pruritus is a kind of clinical symptoms of various skin disease, shows as mainly that skin is itched, macule, pimple, in addition occur oozing out, vesicle, chronic phase, pachyderma can occur and the lichen sample changes.The reason that causes skin pruritus is a lot, as infection, food or drug allergy, the long-pending heat of gastrointestinal tract, dyspepsia, endocrine disturbance and multisystem disease etc.
The treatment skin pruritus should cause clearly at first what the factor of pruritus is, avoids, dispels the cause of disease, and anti symptom treatment can have good effect again.The treatment skin pruritus is used Western medicine antihistaminic, calcium preparation and hormone etc. always at present.Because these medicine contraindications are many, often cause drowsiness, weak and other side reactions, influence patient's orthobiosis and work, chronic patient is difficult to adhere to treatment.Clinical practice proves that motherland's tradition Chinese medicine is delayed the chronic of outbreak repeatedly with its safety, conditioning property and its distinctive feature to treatment skin pruritus, the especially course of disease, and effect is fine.
The traditional Chinese medical science thinks, ailment said due to cold or exposure, damp, pathogenic heat, blood deficiency, worm are excessive etc. is morbific main cause, and treatment should be a principle with dispelling wind damp eliminating, heat-clearing and toxic substances removing, blood enriching and dryness moistening, blood circulation promoting and blood stasis dispelling, sets upright antipruritic effect to reach to get rid of evils.The oral Chinese medicine preparation that is used for the treatment of skin pruritus in the market seldom, and curative effect is not remarkable mostly, so provide a kind of evident in efficacy, definite Chinese medicine preparation to be very important.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition for the treatment of skin pruritus;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method for the treatment of skin pruritus;
The object of the invention also is to provide a kind of method of quality control for the treatment of the Chinese medicine composition of skin pruritus.
The present invention seeks to be achieved through the following technical solutions:
The Chinese medicine composition of treatment skin pruritus of the present invention is to be made by the crude drug of following weight ratio:
Fructus Xanthii (stir-fry, deburring) 150-320 weight portion Fructus Atriplicis Sibiricae 180-280 weight portion
Rhizoma Chuanxiong 180-320 weight portion Semen Persicae 100-240 weight portion Herba Solani Lyrati 50-180 weight portion;
The Chinese medicine composition of treatment skin pruritus of the present invention can be made by the crude drug of following weight ratio:
Fructus Xanthii (stir-fry, deburring) 150-320 weight portion Fructus Kochiae 180-280 weight portion
Rhizoma Chuanxiong 180-320 weight portion Flos Carthami 100-240 weight portion Herba Solani Lyrati 50-180 weight portion;
The above-mentioned raw materials optimum ratio is:
Fructus Xanthii (stir-fry, deburring) 260-300 weight portion Fructus Kochiae 220-260 weight portion
Rhizoma Chuanxiong 230-280 weight portion Flos Carthami 120-160 weight portion Herba Solani Lyrati 60-90 weight portion;
The above-mentioned raw materials optimum ratio is:
Fructus Xanthii (stir-fry, deburring) the 270 weight portion Fructus Kochiae, 220 weight portions
Rhizoma Chuanxiong 250 weight portion Flos Carthamis 130 weight portion Herba Solani Lyratis 70 weight portions;
The above-mentioned raw materials optimum ratio is:
Fructus Xanthii (stir-fry, deburring) the 290 weight portion Fructus Kochiae, 250 weight portions
Rhizoma Chuanxiong 240 weight portion Flos Carthamis 120 weight portion Herba Solani Lyratis 70 weight portions;
Compositions of the present invention technology adding adjuvant is routinely made clinical acceptable forms such as tablet, capsule, oral liquid, drop pill, spray, granule; Described adjuvant comprises solvent, disintegrating agent, correctives, antiseptic, coloring agent, binding agent, lubricant, substrate etc.
The preparation method of Chinese medicinal composition granules of the present invention is:
Method for making: crude drug decocts with water 2-3 time, and each 1-3 hour, collecting decoction staticly settled 7-9 hour, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃); 1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, drying, promptly.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) thin layer of Rhizoma Chuanxiong is differentiated
Get present composition granule 18g, add dehydrated alcohol 50ml, supersound process 25-35 minute, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 40-55 hour, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-dioxane-acetic acid (85-95: 20-30: 3-5) be developing solvent, launch, take out, dry, put under the uviol 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;
(2) thin layer of the Fructus Kochiae is differentiated
Get present composition granule 18g, add dehydrated alcohol 70ml, jolting was extracted 25-35 minute, filter, filtrate adds hydrochloric acid 4ml, and water-bath backflow 8-12 minute is concentrated into about 5ml then, add water 10ml, 60ml divides 2-4 extraction, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (8-12: 0.2-0.7) be developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (20-30: 70-80: 1-2) be mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing ferulic acid, add methanol-formic acid (90-98: mixed solution 3-7), make the solution that contains 8ug among every 1ml, filter with microporous filter membrane (0.45um), promptly;
The preparation of need testing solution: it is an amount of to get under the present composition granule content uniformity granule, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, (90-98: mixed solution 25ml 4-6) claims to decide weight, supersound process 25-35 minute accurate adding methanol-formic acid, put cold, claim to decide weight, (90-98: mixed solution 4-6) shakes up after supplying the weight that subtracts mistake with methanol-formic acid again, filter with microporous filter membrane (0.45um), promptly; Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.
Pharmaceutical composition method of quality control of the present invention is preferably as follows one or more in discrimination method and/or the assay:
Differentiate:
(1) thin layer of Rhizoma Chuanxiong is differentiated
Get present composition granule 18g, add dehydrated alcohol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 48 hours, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-dioxane-acetic acid (90: 25: 4), launch, take out, dry, put under the uviol 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;
(2) thin layer of the Fructus Kochiae is differentiated
Get present composition granule 18g, add dehydrated alcohol 70ml, jolting was extracted 30 minutes, filter, filtrate adds hydrochloric acid 4ml, and water-bath refluxed 10 minutes, was concentrated into about 5ml then, add water 10ml, 60ml divides 3 extractions, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (10: 0.5) is developing solvent, launches, and takes out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (25: 75: 1.8) is a mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing ferulic acid, adds the mixed solution of methanol-formic acid (95: 5), makes the solution that contains 8ug among every 1ml, filters with microporous filter membrane (0.45um), promptly;
It is an amount of that granule is got under the present composition granule content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds methanol-formic acid (95: 5) claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minutes, put coldly, claim to decide weight again, after supplying the weight that subtracts mistake with the mixed solution of methanol-formic acid (95: 5), shake up, filter with microporous filter membrane (0.45um), promptly; Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.
The present composition has good drug effect, compares existing preparation and shows better drug effect.The method of quality control of Chinese medicine composition provided by the present invention, be by obtaining behind the creative experiment sieving of big measuring, pass through screening in the discrimination method to sample treatment, the selection of developing solvent, make and differentiate that specificity is fine, and method is economic and practical, the result is quick, and can both use different lamellaes.Pass through screening in the content assaying method to sample, test sample processing method, the selection of developing solvent, make content assaying method effectivelyly to carry out quality control, and will compare more stable that product that additive method measures shows on pharmacological effect with the product that this method is measured to product.
The specific embodiment
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 pharmacological testing
Medicine group I Fructus Xanthii of the present invention (stir-fry, deburring) 190g Fructus Atriplicis Sibiricae 180g Rhizoma Chuanxiong 190g Semen Persicae 180g Herba Solani Lyrati 100g;
Medicine group II Fructus Xanthii of the present invention (stir-fry, deburring) 290g Fructus Kochiae 250g Rhizoma Chuanxiong 240g Flos Carthami 120g Herba Solani Lyrati 70g
Medicine group III Fructus Xanthii of the present invention (stir-fry, deburring) 270g Fructus Kochiae 220g Rhizoma Chuanxiong 250g Flos Carthami 130g Herba Solani Lyrati 70g
Medicine group IV Fructus Xanthii of the present invention (stir-fry, deburring) 200g Fructus Kochiae 200g Rhizoma Chuanxiong 200g Flos Carthami 200g Herba Solani Lyrati 100g
The commercially available wind-repellent itching-relieving granules of positive controls
Prescription according to above four groups of medicines of the present invention is prepared into granule, and relatively the reliability of curative effect of medication of the present invention is determined in the antipruritic and effect of invigorating blood circulation between each group.
1, itching-relieving action:
Medicinal granule of the present invention causes 60 Cavia porcelluss that influence of the reaction of itching to histamine phosphate, body weight (300 ± 30) g, male and female half and half, be divided into 6 groups at random, abrade right back instep depilation place, the concentration 0.1ml/ of local application foot, only drip 0.01 0.05mL/ of histamine phosphate in wound face behind the 10min, after this every 3min with 0.01,0.02,0.03,0.04 ... progressive concentration, later to lick the right back histamine phosphate's total amount that is given when sufficient be itch-threshold Cavia porcellus to occur, the results are shown in following table.
The skin granule of itching causes the influence (x ± s) of the reaction of itching to histamine phosphate
| Group | Dosage (g/kg) | n | Itch-threshold (histamine phosphate's total amount) (μ g) |
| Medicine group I of the present invention | 3 | 10 | 247.6±58.4**△△☆ |
| Medicine group II of the present invention | 3 | 10 | 239.8±61.2**△△☆ |
| Medicine group III of the present invention | 3 | 10 | 243.4±59.2**△△☆ |
| Medicine group IV of the present invention | 3 | 10 | 213.5±71.4**△ |
| Positive controls | 6 | 10 | 165.5±74.8** |
| Negative control group | - | 10 | 71.0±36.2 |
* and negative control group be P＜0.001 relatively, and △ △ and positive controls be P＜0.01 relatively, and △ and positive controls be P＜0.05 relatively, and ☆ and medicine group IV compare＜0.05.
The result shows: medicinal granule of the present invention and wind-repellent itching-relieving granules and negative control group compare, and histamine phosphate is caused the reaction of itching all the obvious suppression effect.Medicinal granule of the present invention and positive controls granule compare, and itching-relieving action has significance to improve.The itching-relieving action of medicine group I of the present invention, II, III is significantly higher than medicine IV of the present invention, and does not have significant difference between the medicine group I of the present invention, II, III.
2, the effect of invigorating blood circulation:
Select 48 of 20～24 monthly age Wistar male rats for use, body weight (550 ± 56) g is divided into the wind-repellent itching-relieving granules group at random, medicine group I of the present invention, II, III, IV and old model group, more than be divided into 6 groups, 8 every group, irritate stomach respectively every day and give medicine group 3gkg of the present invention
-1, aspirin 5.5mgkg
-1, 22d behind the last administration 1h, through carotid artery blood sampling type 3ml, adds 3.8 sodium citrate solution anticoagulants (1: 9) in plastic tube continuously, mixing, and 2h is interior with 1000rmin
-1Centrifugal 10min, platelet blood plasma (RRP) and sucking-off are rich in preparation, and remainder is with 3000rmin
-1Centrifugal 15min gets platelet-poor plasma (PPP), and ADP is a derivant, measures 1min platelet aggregation rate [PAG (1)], 5min platelet aggregation rate [PAG (5)], maximum agglutination rate [PAG (M)] with TYXN291 intelligence blood agglutometer.Experimental result sees Table
To platelet aggregation influence (
-X ± s) (n=8)
Annotate: * P＜0.01 is compared with model group; △ P＜0.01 is compared with the wind-repellent itching-relieving granules group; ☆ P＜0.05 is compared with medicine group IV.
The result shows: medicine of the present invention and wind-repellent itching-relieving granules be to the influence of rat platelet aggregation function, and comparing with model group all has significant difference.Medicine of the present invention and wind-repellent itching-relieving granules relatively also have significant difference to the influence of platelet aggregation.Between medicine group I of the present invention, II, III and the medicine group IV of the present invention significant difference is arranged more also, and there was no significant difference between the medicine group I of the present invention, II, III.
The experiment of experimental example 2 assays
Through a large amount of experimental studies, determine to adopt the content of ferulic acid in the high-efficient liquid phase color popularize law mensuration medicine of the present invention, to improve the quality determining method of medicine of the present invention.Part test the results are shown in down:
1, the preparation of need testing solution
1. extract the preferred of solvent
It is an amount of to get medicament composition granule agent of the present invention, porphyrize, and precision takes by weighing about 3g respectively, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds the methanol-formic acid of different mixing proportion claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minute, put coldly, supply the weight that subtracts mistake, after the more different identical times of proportioning solvent extraction, content of ferulic acid wherein the results are shown in following table:
| Solvent burden ratio (methanol: formic acid) | 90∶5 | 93∶5 | 95∶5 | 98∶5 |
| Ferulaic acid content (mg/g) | 0.034 | 0.038 | 0.057 | 0.041 |
As can be seen from the above table, the mixed proportion of methanol-formic acid is 95: 5 o'clock, and the ferulaic acid content that records is the highest.
2. the selection of supersound extraction time
Get medicinal granule of the present invention, porphyrize is got 4 parts of equivalent, the mixed solution that adds methanol-formic acid, supersound process (power 250W, frequency 40KHZ) is 10,20,30,40 minutes respectively, put coldly, content of ferulic acid in the solution of relatively more different extraction times the results are shown in following table:
| Extraction time (min) | 10 | 20 | 30 | 40 |
| Ferulaic acid content (mg/g) | 0.021 | 0.038 | 0.057 | 0.056 |
Above result shows that supersound extraction can be extracted ferulic acid fully in 30 minutes.
2, the selection of mobile phase
Having chosen and having prepared the more approaching methanol-water-glacial acetic acid of solvent with test sample is mobile phase, has compared the chromatographic peak separating effect under different proportionings, the results are shown in following table:
| The developing solvent proportioning | 20∶70∶1 | 20∶75∶2 | 25∶75∶1.8 | 30∶80∶1.8 |
| The chromatographic peak separating effect | Difference | Difference | Good | Very poor |
As can be seen from the above results, the proportioning of mobile phase methanol-water-glacial acetic acid is 25: 75: 1.8 o'clock, and the chromatographic peak separating effect is best, and it is unclear separation to occur, and main peak has phenomenons such as interference.
3, the methodological study of assay:
To adopting ferulaic acid content in the high effective liquid chromatography for measuring pharmaceutical preparation of the present invention, also carried out a large amount of methodological investigations tests, with the stability of determining this method, repeatability etc., part test as follows:
(1) stability test reference substance solution respectively at preparing the back 0,2,4,6,12,24 hour, is measured in accordance with the law, and the result shows that it is basicly stable in 24 hours, the results are shown in following table
(2) linear relationship is investigated and to be got reference substance solution (0.01052mg/ml) and shake up, accurate respectively 1,3,5,7,9, the 11 μ l of absorption inject high performance liquid chromatograph, measure peak area, the results are shown in following table, and drawing standard curve, show that ferulic acid is linear between 0.01052 μ g-0.11572 μ g, its regression equation is:
Area＝4153.9435×Amt+7.7814(r＝0.9996)
(3) the accurate need testing solution 10 μ l that draw of precision test repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the results are shown in following table:
(4) the text method is pressed in the repeatability test, gets 5 parts in medicinal granule sample of the present invention, measures respectively, tries to achieve relative standard deviation＜2%, the results are shown in following table:
(5) the recovery test precision takes by weighing accurate respectively again ferulic acid reference substance solution (16.832ug/ml) 10ml that adds of sample 3.0g of the medicinal granule of the present invention of known content, preparation method operation by above need testing solution, measure its content, and calculate its response rate, measurement result sees the following form:
4, according to the preparation method of medicinal granule of the present invention, carried out pilot plant test, and will be wherein three batches detect according to quality determining method of the present invention, the result shows, can effectively control pharmaceutical preparation quality of the present invention with quality determining method of the present invention, guarantee stability, the reliability of curative effect of medication of the present invention.
Experimental example 3 identification experiments
1) thin layer of Rhizoma Chuanxiong is differentiated
1. the preparation of need testing solution
A, extraction choice of Solvent are got totally 4 parts of medicinal granule 18g of the present invention, add 50% ethanol, 75% ethanol, 95% ethanol, each 50ml of dehydrated alcohol respectively, supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution.The fluorescence speckle color developing effect of more different need testing solutions on lamellae the results are shown in following table:
| Extract solvent | 50% ethanol | 75% ethanol | 95% ethanol | Dehydrated alcohol |
| Color developing effect | The speckle color developing effect is very poor, and interference is arranged | The speckle color developing effect is poor, and interference is arranged | The speckle color developing effect is poor, and interference is arranged | Color developing effect is good |
Totally 4 parts of medicinal granule 18g of the present invention are got in the selection of b, extraction time, add each 50ml of dehydrated alcohol, and supersound process 10,20,30,40 minutes is filtered, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution.The fluorescence speckle color developing effect of more different need testing solutions on lamellae the results are shown in following table:
| Ultrasonic time | 10min | 20min | 30min | 40min |
| Color developing effect | There is not the colour developing speckle | The speckle colour developing is shallow | Color developing effect is good | Identical with the 30min effect |
From above result of the test as can be seen, add dehydrated alcohol, the need testing solution that supersound process 30min is prepared, fluorescence speckle color developing effect is good on lamellae, the Pass Test requirement.
2. the preparation of sample solution
Get totally four parts of Rhizoma Chuanxiong control medicinal material 1g, add dehydrated alcohol 30ml dipping 24,48,72 hours and supersound extraction 30min, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast.Compared the employing Different Extraction Method, the fluorescence speckle color developing effect of reference substance solution on lamellae the results are shown in following table:
| Extracting method | Dipping 24h | Dipping 48h | Dipping 72h | Ultrasonic 30min |
| Color developing effect | The speckle colour developing is very shallow | The speckle color developing effect is good | The speckle color developing effect is good | The speckle colour developing is shallow |
As can be seen from the above results, the Rhizoma Chuanxiong control medicinal material adds the dehydrated alcohol dipping control medicinal material solution that 48h extracted, and the fluorescence speckle color developing effect on lamellae is good, the Pass Test requirement.
The selection of 3. developing solvent proportioning
Draw totally four parts of need testing solution, each 15 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with benzene-dioxane-acetic acid is developing solvent, proportioning was respectively 85: 20: 3,90: 20: 3,90: 25: 4,95: 25: 4, launch, airing is put under the uviol lamp (365nm) and is observed.Observe the unfolded effect of each fluorescence speckle of test sample on the lamellae, the results are shown in following table:
| The developing solvent proportioning | 85∶20∶3 | 90∶20∶3 | 90∶25∶4 | 95∶25∶4 |
| Each speckle launches effect | Separate badly, disturb big | Separate badly, interference is arranged | Good separating effect, noiseless | Separate badly, disturb big |
Developing solvent proportioning as can be seen from the above table is 90: 25: 4 o'clock, launches effectively on lamellae, is fit to test requirements document.
4. the selection of point sample amount
Draw need testing solution 1 μ l, 5 μ l, 10 μ l, 15 μ l, each 15 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with benzene-dioxane-acetic acid (90: 25: 4) is developing solvent, launch, airing is put under the uviol lamp (365nm) and is observed, observe the effect of test sample fluorescence speckle colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 1μl | 5μl | 10μl | 15μl |
| Effect | Test sample does not have the fluorescence speckle in corresponding reference substance position | Test sample is in corresponding reference substance position fluorescence speckle very slight color | Test sample is of light color at corresponding reference substance position fluorescence speckle | Test sample is good at corresponding reference substance position fluorescence speckle color developing effect |
Test sample point sample amount is when 15 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
5. negative control test
Get the negative sample that lacks Rhizoma Chuanxiong, prepare negative control solution, launch the back and corresponding fluorescence speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned discrimination method.
2) thin layer of the Fructus Kochiae is differentiated
1. the preparation of need testing solution
A, get medicinal granule 18g of the present invention, add dehydrated alcohol 70ml, jolting was extracted 10,20,30,40 minutes, filter, filtrate adds hydrochloric acid 4ml, and water-bath refluxed 5,8,10,12 minutes, was concentrated into about 5ml then, add water 10ml, 60ml divides 3 extractions, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 2ml, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution.Compare difference extraction time gained need testing solution, the color developing effect on lamellae the results are shown in following table:
As can be seen from the above table, add the dehydrated alcohol jolting and extract 30min, filter, filtrate adds hydrochloric acid 4ml, after water-bath refluxed 10 minutes, and prepared need testing solution Pass Test requirement, color developing effect is good on lamellae, and compares with other each extracting method and to have saved test period.
B, by the extracting solution that above-mentioned preferred extracting method makes, be concentrated into about 5ml, add water 10ml, 60ml extracts respectively 2 times, 3 times and 4 times with petroleum ether (60-90 ℃), combined ether liquid, evaporate to dryness, residue add dehydrated alcohol 2ml, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution.More different extraction times, the need testing solution color developing effect on lamellae the results are shown in following table:
| Extraction times | 2 times | 3 times | 4 times |
| Color developing effect | The speckle colour developing is shallow slightly | The speckle colour developing is clear, noiseless. | Effect is identical when extracting 3 times |
As can be seen from the above table, 3 gained need testing solutions of petroleum ether extraction, 4 color developing effects of color developing effect on lamellae and extraction are identical, so extract 3 Pass Test requirements.
The selection of 2. developing solvent proportioning
Drawing above-mentioned need testing solution 25 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, is developing solvent with the chloroform-methanol, proportioning was respectively 5: 1,10: 1,10: 0.5,40: 1.5, launched airing, spray phosphomolybdic acid test solution, it is clear that hot blast blows to the speckle colour developing.Compare the effect of test sample development of chromatogram, the results are shown in following table:
| The developing solvent proportioning | 5∶1 | 10∶1 | 10∶0.5 | 40∶1.5 |
| Each speckle launches effect | Separate badly, disturb big | Separate badly, disturb big | Good separating effect, noiseless | Separate badly, thanks for your hospitality big |
Developing solvent proportioning as can be seen from the above table is 10: 0.5 o'clock, launches effectively on lamellae, is fit to test requirements document.
3. the selection of point sample amount
Drawing above-mentioned need testing solution 5 μ l, 10 μ l, 15 μ l, 20 μ l, 25 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, is developing solvent with chloroform-methanol (10: 0.5), launch, airing, spray phosphomolybdic acid test solution, it is clear that hot blast blows to the speckle colour developing.Observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 5μl | 10μl | 15μl | 20μl | 25μl |
| Effect | Test sample is at corresponding reference substance position immaculate | Test sample is at corresponding reference substance position immaculate | Test sample is very shallow in corresponding reference substance position spot colors | Test sample is shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 25 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4. negative control test
Get the negative sample that lacks the Fructus Kochiae, prepare negative control solution, launch the back and corresponding fluorescence speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned discrimination method.
The specific embodiment
Following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment 1: granule
Fructus Xanthii (stir-fry, deburring) 190g Fructus Atriplicis Sibiricae 180g
Rhizoma Chuanxiong 190g Semen Persicae 180g Herba Solani Lyrati 100g;
The above five tastes decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃).1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, drying, promptly.
Embodiment 2: effervescent tablet
Fructus Xanthii (stir-fry, deburring) 240g Fructus Tribuli 230g
Rhizoma Chuanxiong 190g Semen Persicae 190g Herba Solani Lyrati 100g;
The above five tastes decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃), concentrated, and vacuum drying is pulverized.After the Polyethylene Glycol fusion, add sodium bicarbonate. stir. cooling is pulverized, and crosses 80 mesh sieves.In addition citric acid, sweetener are crossed 80 mesh sieves, with medicated powder, Polyethylene Glycol wrappage fine powder mixing, alcohol granulation, drying, granulate, tabletting, promptly.
Embodiment 3: soft capsule
Fructus Xanthii (stir-fry, deburring) 300g Fructus Kochiae 250g
Rhizoma Chuanxiong 240g Flos Carthami 170g Herba Solani Lyrati 50g;
The above five tastes decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, get the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃), vacuum drying is crushed to 120～150 orders, adds an amount of vegetable oil mix homogeneously, add an amount of suspending agent again, evenly, be pressed into soft capsule.Soft capsule material is made of according to a certain percentage gelatin, G ﹠ W.
Embodiment 4: oral liquid
Fructus Xanthii (stir-fry, deburring) 220g Fructus Kochiae 230g Rhizoma Chuanxiong 240g
Flos Carthami 190g English 100g
The above five tastes decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, get supernatant concentration to an amount of, other gets sucrose and makes syrup in right amount, merges with above-mentioned medicinal liquid, it is an amount of to add correctives and antiseptic, adjusts total amount to 1000ml, stirs evenly, filter, embedding, sterilization, promptly.
Embodiment 5: capsule
Fructus Xanthii (stir-fry, deburring) 290g Fructus Kochiae 250g
Rhizoma Chuanxiong 240g Flos Carthami 120g Herba Solani Lyrati 70g;
The above five tastes decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction, staticly settled 8 hours, and got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃), vacuum drying is pulverized, and mixes with an amount of dextrin, starch, granulate, drying incapsulates, promptly.
Embodiment 6: granule
Fructus Xanthii (stir-fry, deburring) 270g Fructus Kochiae 220g
Rhizoma Chuanxiong 250g Flos Carthami 130g Herba Solani Lyrati 70g;
The above five tastes decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃).1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, drying, promptly.
Method of quality control:
Differentiate:
Get this product 18g, add dehydrated alcohol 70ml, jolting was extracted 30 minutes, filtered, and filtrate adds hydrochloric acid 4ml, water-bath refluxed 10 minutes, was concentrated into about 5ml then, added water 10ml, and 60ml divides 3 extractions with petroleum ether (60-90 ℃), combined ether liquid, evaporate to dryness, residue add dehydrated alcohol 1ml, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution.According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (10: 0.5) is developing solvent, launches, and takes out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (25: 75: 1.8) is a mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing ferulic acid, adds the mixed solution of methanol-formic acid (95: 5), makes the solution that contains 8ug among every 1ml, filters with microporous filter membrane (0.45um), promptly.
It is an amount of that granule is got under this product content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds methanol-formic acid (95: 5) claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minutes, put coldly, claim to decide weight again, after supplying the weight that subtracts mistake with the mixed solution of methanol-formic acid (95: 5), shake up, filter with microporous filter membrane (0.45um), promptly.
Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.This product contains Rhizoma Chuanxiong with ferulic acid (C for every bag
10H
10O
4) meter, must not be less than 0.30mg.
Embodiment 7:
Fructus Xanthii (stir-fry, deburring) 200g Fructus Kochiae 200g Rhizoma Chuanxiong 200g
Flos Carthami 200g Herba Solani Lyrati 100g
Method for making: the above five tastes, decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃).1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, and drying is made 720g, promptly.
Differentiate:
(1) get this product 2g, add water 20ml dissolving, strong jolting 1 minute produces a large amount of persistent foams.
(2) get this product 10g, porphyrize adds petroleum ether (30～60 ℃) 20ml, and is airtight, placed 10 hours, jolting is constantly left standstill, after getting supernatant and volatilizing, residue adds methanol 1～2ml dissolving, add 2%3, each 2～3 of the methanol saturated solutions of the methanol solution of 5-dinitrobenzoic acid and potassium hydroxide show light red.
(3) get this product 18g, add dehydrated alcohol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution.Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 48 hours, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 15 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-dioxane-acetic acid (90: 25: 4), launches, take out, dry, put under the uviol 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.
(4) get this product 18g, add dehydrated alcohol 70ml, jolting was extracted 30 minutes, filter, filtrate adds hydrochloric acid 4ml, and water-bath refluxed 10 minutes, was concentrated into about 5ml then, add water 10ml, 60ml divides 3 extractions, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution.According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (10: 0.5) is developing solvent, launches, and takes out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (25: 75: 1.8) is a mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing ferulic acid, adds the mixed solution of methanol-formic acid (95: 5), makes the solution that contains 8ug among every 1ml, filters with microporous filter membrane (0.45um), promptly.
It is an amount of that granule is got under this product content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds methanol-formic acid (95: 5) claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minutes, put coldly, claim to decide weight again, after supplying the weight that subtracts mistake with the mixed solution of methanol-formic acid (95: 5), shake up, filter with microporous filter membrane (0.45um), promptly.
Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.This product contains Rhizoma Chuanxiong with ferulic acid (C for every bag
10H
10O
4) meter, must not be less than 0.30mg.
Function with cure mainly: be used for skin pruritus, urticaria.
Usage and consumption: boiled water is taken after mixing it with water, one time 1～2 bag, 3 times on the one.
Attention: be not taken by pregnant women the careful usefulness of digestive tract ulcer patient.
Specification: every packed 9g.
Claims (9)
1. pharmaceutical composition for the treatment of skin pruritus is characterized in that the crude drug of this pharmaceutical composition consists of:
Fructus Xanthii (stir-fry, deburring) 150-320 weight portion Fructus Atriplicis Sibiricae 180-280 weight portion
Rhizoma Chuanxiong 180-320 weight portion Semen Persicae 100-240 weight portion Herba Solani Lyrati 50-180 weight portion.
2. pharmaceutical composition as claimed in claim 1 is characterized in that in the crude drug composition in this pharmaceutical composition:
Fructus Xanthii (stir-fry, deburring) 150-320 weight portion Fructus Kochiae 180-280 weight portion
Rhizoma Chuanxiong 180-320 weight portion Flos Carthami 100-240 weight portion Herba Solani Lyrati 50-180 weight portion.
3. pharmaceutical composition as claimed in claim 2 is characterized in that the crude drug of this pharmaceutical composition consists of:
Fructus Xanthii (stir-fry, deburring) 260-300 weight portion Fructus Kochiae 220-260 weight portion
Rhizoma Chuanxiong 230-280 weight portion Flos Carthami 120-160 weight portion Herba Solani Lyrati 60-90 weight portion.
4. pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug of this pharmaceutical composition consists of:
Fructus Xanthii (stir-fry, deburring) the 270 weight portion Fructus Kochiae, 220 weight portions
Rhizoma Chuanxiong 250 weight portion Flos Carthamis 130 weight portion Herba Solani Lyratis 70 weight portions.
5. pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug of this pharmaceutical composition consists of:
Fructus Xanthii (stir-fry, deburring) the 290 weight portion Fructus Kochiae, 250 weight portions
Rhizoma Chuanxiong 240 weight portion Flos Carthamis 120 weight portion Herba Solani Lyratis 70 weight portions.
6. as the described preparation of drug combination method of claim 1-5, it is characterized in that this method is:
Crude drug decocts with water 2-3 time, and each 1-3 hour, collecting decoction staticly settled 7-9 hour, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃); 1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, drying, promptly.
7. as the method for quality control of the described pharmaceutical composition of claim 1-5, it is characterized in that this method of quality control comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) get present composition granule 18g, add dehydrated alcohol 50ml, supersound process 25-35 minute, filter, filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 40-55 hour, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-dioxane-acetic acid (85-95: 20-30: 3-5) be developing solvent, launch, take out, dry, put under the uviol 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;
(2) get present composition granule 18g, add dehydrated alcohol 70ml, jolting was extracted 25-35 minute, filter, filtrate adds hydrochloric acid 4ml, and water-bath backflow 8-12 minute is concentrated into about 5ml then, add water 10ml, 60ml divides 2-4 extraction, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (8-12: 0.2-0.7) be developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (20-30: 70-80: 1-2) be mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing ferulic acid, add methanol-formic acid (90-98: mixed solution 3-7), make the solution that contains 8ug among every 1ml, filter with microporous filter membrane (0.45um), promptly;
The preparation of need testing solution: it is an amount of to get under the present composition granule content uniformity granule, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, (90-98: mixed solution 25ml 4-6) claims to decide weight, supersound process 25-35 minute accurate adding methanol-formic acid, put cold, claim to decide weight, (90-98: mixed solution 4-6) shakes up after supplying the weight that subtracts mistake with methanol-formic acid again, filter with microporous filter membrane (0.45um), promptly; Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.
8. the method for quality control of pharmaceutical composition as claimed in claim 7 is characterized in that this method of quality control comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) get present composition granule 18g, add dehydrated alcohol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 48 hours, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-dioxane-acetic acid (90: 25: 4), launch, take out, dry, put under the uviol 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;
(2) get present composition granule 18g, add dehydrated alcohol 70ml, jolting was extracted 30 minutes, filter, filtrate adds hydrochloric acid 4ml, and water-bath refluxed 10 minutes, was concentrated into about 5ml then, add water 10ml, 60ml divides 3 extractions, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (10: 0.5) is developing solvent, launches, and takes out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (25: 75: 1.8) is a mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing ferulic acid, adds the mixed solution of methanol-formic acid (95: 5), makes the solution that contains 8ug among every 1ml, filters with microporous filter membrane (0.45um), promptly;
It is an amount of that granule is got under the present composition granule content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds methanol-formic acid (95: 5) claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minutes, put coldly, claim to decide weight again, after supplying the weight that subtracts mistake with the mixed solution of methanol-formic acid (95: 5), shake up, filter with microporous filter membrane (0.45um), promptly; Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.
9. the method for quality control of pharmaceutical composition as claimed in claim 8 is characterized in that this method of quality control comprises following method:
Choose following material medicine and make granule:
Fructus Xanthii (stir-fry, deburring) the 200 weight portion Fructus Kochiae, 200 weight portions
Rhizoma Chuanxiong 200 weight portion Flos Carthamis 200 weight portion Herba Solani Lyratis 100 weight portions;
The above five tastes decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction staticly settled 8 hours, got the clear paste that supernatant concentration to relative density is 1.36 (65～75 ℃).1 part of qinghuo reagent adds 3 parts of cane sugar powders, and 1 part in dextrin and ethanol are an amount of, make granule, are drying to obtain.
Method of quality control comprises to be differentiated and assay:
Differentiate:
(1) get this product 18g, add dehydrated alcohol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds dehydrated alcohol 30ml dipping 48 hours, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 2ml dissolving, medical material solution in contrast; According to the thin layer chromatography test, draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-dioxane-acetic acid (90: 25: 4), launch, take out, dry, put under the uviol 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;
(2) get this product 18g, add dehydrated alcohol 70ml, jolting was extracted 30 minutes, filter, filtrate adds hydrochloric acid 4ml, and water-bath refluxed 10 minutes, was concentrated into about 5ml then, add water 10ml, 60ml divides 3 extractions, combined ether liquid, evaporate to dryness with petroleum ether (60-90 ℃), residue adds dehydrated alcohol 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol, makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel G plate, with chloroform-methanol (10: 0.5) is developing solvent, launches, and takes out, dry, spray is with the phosphomolybdic acid test solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
According to high effective liquid chromatography for measuring: chromatographic condition and system suitability test are filler (4.6 * 150mm, 5 μ m) with octadecylsilane chemically bonded silica; Methanol-water-glacial acetic acid (25: 75: 1.8) is a mobile phase; The detection wavelength is 330nm, and theoretical cam curve is calculated by ferulic acid should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing ferulic acid, adds the mixed solution of methanol-formic acid (95: 5), makes the solution that contains 8ug among every 1ml, filters with microporous filter membrane (0.45um), promptly;
It is an amount of that granule is got under this product content uniformity in the preparation of need testing solution, porphyrize, and precision takes by weighing about 3g, put in the tool plug Erlenmeyer flask, the accurate mixed solution 25ml that adds methanol-formic acid (95: 5) claims to decide weight, supersound process (power 250W, frequency 40KHZ) 30 minutes, put coldly, claim to decide weight again, after supplying the weight that subtracts mistake with the mixed solution of methanol-formic acid (95: 5), shake up, filter with microporous filter membrane (0.45um), promptly; Accurate respectively reference substance liquid, each the 10 μ l injection chromatograph of liquid of test sample liquid drawn of assay method measured, promptly.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100647986A CN101274037B (en) | 2007-03-27 | 2007-03-27 | Detection method of composition for curing skin pruritus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100647986A CN101274037B (en) | 2007-03-27 | 2007-03-27 | Detection method of composition for curing skin pruritus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104688832A (en) * | 2013-12-04 | 2015-06-10 | 青岛永通电梯工程有限公司 | Traditional Chinese medicine composition ointment for relieving itching |
| CN110967440A (en) * | 2018-09-28 | 2020-04-07 | 九芝堂股份有限公司 | Method for identifying belvedere fruit in oral liquid containing donkey-hide gelatin, pearl essence and blood |
| CN113892646A (en) * | 2021-10-19 | 2022-01-07 | 吉林省华侨药业集团有限公司 | Preparation process of granular preparation for treating skin itch and whole-granule sieving device thereof |
-
2007
- 2007-03-27 CN CN2007100647986A patent/CN101274037B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104688832A (en) * | 2013-12-04 | 2015-06-10 | 青岛永通电梯工程有限公司 | Traditional Chinese medicine composition ointment for relieving itching |
| CN110967440A (en) * | 2018-09-28 | 2020-04-07 | 九芝堂股份有限公司 | Method for identifying belvedere fruit in oral liquid containing donkey-hide gelatin, pearl essence and blood |
| CN113892646A (en) * | 2021-10-19 | 2022-01-07 | 吉林省华侨药业集团有限公司 | Preparation process of granular preparation for treating skin itch and whole-granule sieving device thereof |
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| Publication number | Publication date |
|---|---|
| CN101274037B (en) | 2011-08-17 |
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