Medical network - February 17 state pharmacopoeia committee issued "about < China pharmacopoeia > 2015 a quasi quality publication of the revised standard varieties", "Chinese pharmacopoeia" 2015 version of the film contains varieties to quality standard revision of the four varieties announces, standard public date for 3 months.
It is understood that the public plan quality standard revision of the four varieties of scutellaria baicalensis extract, motherwort cream, herba leonuri particle, WJH bezoar sedative bolus.
1, scutellaria baicalensis georgi extract
Huangqin Tiquwu
SCUTELLARIA EXTRACT
[method] taking radix scutellariae, add water decoction, merging decoction, to concentrate right amount, using hydrochloric acid to adjust pH value to 1.0 ~ 1.0, 80 ℃ heat and let stand, filtration, precipitates with right amount water beaten, adjust pH value to 7.0 with 40% sodium hydroxide solution, add an equal amount of ethanol, stir to dissolve and filtration, the filtrate hydrochloric acid to adjust pH value to 1.0 ~ 1.0, 60 ℃ heat and let stand, filtration, sedimentation, in turn, with a moderate amount of water and different concentrations of ethanol washing to neutral, and ethanol, decompression drying, for a quick.
2, good mother grass cream
Yimucao Gao
This product is made of herba leonuri processed to Fried paste.
【 method 】 take motherwort, chopped, add water decoction twice, each time 2 hours, merging decoction, filtration, the filtrate to concentrate relative density is 1.21 ~ 1.25 (80 ℃) cream. Per 100 g fresh cream add brown sugar 200 g, heating, melting blending, concentrated to the regulation of relative density, quick.
【 characteristics 】 this product is dark brown thick semi-fluid; Micro, bitter, sweet taste.
[identify] in [on] content of chromatograph chart, the chromatogram of the test should be rendered in consistent with that of reference substance chromatographic peak retention time of chromatographic peak.
"Check" relative density should be not less than 1.36 the general principles of the (0183).
Other should comply with the relevant Fried preparation under the provisions of the general principles of the (0183).
According to content determination 】 【 HPLC determination of the general principles of the (0512).
The chromatographic conditions and system suitability test With strong cation exchange bonded silica gel as the filling agent; With acetonitrile - 0.05 mol/L of potassium dihydrogen phosphate solution - phosphate (thus 5-0. 15) as mobile phase; Detection wavelength of 192 nm. Theoretical plate number calculated by hydrochloric acid alkali water Sue peak should be not less than 2000.
Reference substance solution preparation The right amount of hydrochloric acid alkali water su reference substance, precision said, adding methanol each 1 ml solution containing 0.3 mg, quick.
Take this product preparation of test sample solution, shake well, take about 1 g, precision said, with a plug in the conical flask, precision add 25 ml, 0.5% hydrochloric acid methanol solution according to weight, ultrasonic processing (power 250 w, frequency 33 KHZ) 30 minutes, put the cold, said weight, again with 0.5% hydrochloric acid methanol solution to make up the weight loss reduction, shake well, filtration, take the filtrate, quick.
Measurement precision respectively from the reference substance solution with each 10 mu l solution, injection liquid chromatograph, determination, quick.
This product per 1 g containing hydrochloric acid alkali water Sue (C7H13NO2 · HCl), shall not be less than 3.6 mg.
【 functions and indications 】 activating blood regulate the menstrual function. Used for blood stasis caused by irregular periods, postpartum lochia, see menstrual quantity is little, dripping wet is not net, postpartum hemorrhage, time is too long; Postpartum subinvolution of uterus see the syndrome.
[usage and dosage 】 oral. A 10 g, 1 ~ 2 times a day.
【 note 】 pregnant women are prohibited.
【 specification 】 (1) each containing 120 g (3) (2) each containing 125 g 250 g per bottle
【 storage 】 sealed.
3, herba leonuri particle
Yimucao Keli
Herba leonuri prescription 】 【 1350 g
【 method 】 take motherwort, chopped, add water decoction for 3 hours, Fried fluid filtration, the filtrate to concentrate the relative density of 1.04 (90 ~ 90 ℃) paste, quiet place, take the supernatant, enriching to relative density is 1.36 ~ 1.38 (83 ℃), the thick paste; Or enrichment to relative density is 1.15 ~ 1.18 (50 ℃) paste, clear cream by spray drying into extract powder, add sugar 600 g and the right amount of dextrin, blending, granules, drying, made of 1000 g/specifications (1); Or adding dextrin, stevia sugar right amount; Or adding dextrin, starch in moderation, granules, drying, made of 333 g/specifications (2); Or adding dextrin and starch in moderation, granules, drying, made of 267 g/specifications (3). Or take motherwort, chopped, add water right amount, in 95? Dynamic leaching 3 ℃ for 2 hours, leach liquor by solid-liquid separation, overspeed centrifugal, clear liquid stress concentration to the relative density of 1.10 (50 ℃) clear cream, spray drying into fine powder, dextrin, malt dextrin and stevia right amount, blending, granules, drying, made of 133 g/specifications (4), a quick.
【 characteristics 】 this product is a tan to brown granules; Sweet taste, slightly bitter taste bitter, sweet or bitter (not stevia sugar or sugar cane).
[identify] (1) take this product 5 g/specifications (1), 2 g/specification (2), (3) or 1 g/specifications (4), add boiling water for 30 ml to dissolve, put the cold, centrifugal (3000 RPM), take the supernatant, and by polyamide column (80 ~ 100 mesh, 3 g, wet packing column), 50 ml water elution, abandon to water eluent, reoccupy 50 ml 20% ethanol elution, abandon to 20% ethanol elution liquid, with 50 ml 70% ethanol elution and finally collect the eluent, zhenggan residue add 1 ml dissolved methanol, centrifugal, take that as a solution of the supernatant fluid. Another take motherwort control medicinal material 1 g, 1 hour 50 ml of water is boiling, put the cold, filtration, the filtrate concentrated to around 30 ml, vibration and ethyl acetate extract 2 times, each time 30 ml, combination of ethyl acetate extract, dry, residual methanol 1 ml to dissolve, as a control medicine solution. According to thin layer chromatography (TLC) (0502) general test, 5 mu l learned these two solutions, each point in the same high silica G thin layer plate, ethyl acetate, butanone - formic acid and water (5:3:1:1) as an agent, and taken out, dry spray aluminum chloride ethanol solution at 1%, at 105 ℃ bake for about 5 minutes, examine under ultraviolet light (365 nm). In the chromatogram of the test, chromatographic corresponding to the position, show the same color of the fluorescent spots.
(2) in the "content determination under chromatogram, in the chromatogram of the test should be presented with the reference substance chromatographic peaks corresponding to the retention time of chromatographic peak.
"Check" should comply with the relevant granules under the provisions of the general principles of the (0104)
According to content determination 】 【 HPLC determination of the general principles of the (0512).
The chromatographic conditions and system suitability test With strong cation exchange bonded silica gel as filler (SCX - strong cation exchange resin column); With acetonitrile - 0.05 mol/L of potassium dihydrogen phosphate - phosphate (thus 5-0. 15) as mobile phase; Detection wavelength of 192 nm. Theoretical plate number calculated by hydrochloric acid alkali water su feng, should be not less than 2000.
Reference substance solution preparation The right amount of hydrochloric acid alkali water su reference substance, precision said, adding methanol each 1 ml solution containing 0.1 mg, quick.
Preparation of test sample solution, the load under different amount in the blender, apply adequate amount, fine, take about 1 g/specifications (1), 0.4 g/specification (2), (3)/specification (4), or 0.2 g precision said, with a plug in the conical flask, precision in 0.5% hydrochloric acid methanol solution 25 ml, plug, said weight, ultrasonic processing (power 250 w, frequency 33 KHZ) 30 minutes, put the cold, said weight, again with 0.5% hydrochloric acid methanol solution to make up the weight loss reduction, shake well, filtration, take the filtrate, quick.
Measurement precision respectively from the reference substance solution with each 10 mu l solution, injection liquid chromatograph, determination, quick.
Each bag contains leonurus with hydrochloric acid water Sue alkali (C7H13NO2 · HCl), shall not be less than 27.0 mg.
【 functions and indications 】 activating blood regulate the menstrual function. Used for blood stasis due to menstruation to be not moved, postpartum lochia, see
The less water, dripping wet is not net, postpartum haemorrhage time is too long; Postpartum subinvolution of uterus see the syndrome.
【 usage and dosage 】 water blunt. A 1 bag, 2 times a day.
【 note 】 pregnant women are prohibited.
【 specification 】 15 g per bag (1) (2) (3) 4 g 5 g (4) 2 g (no sugar or stevia sugar)
【 storage 】 sealed
4, WJH bezoar sedative bolus
Wanshi Niuhuang Qingxin Wan
Bezoar prescription 】 【 10 g cinnabar 60 g
Rhizoma coptidis gardenia 200 g 200 g
Radix scutellariae turmeric 80 g 120 g
【 method 】 above the six flavors, in addition to the bezoar, cinnabar water to fly a very fine powder; The rest of the rhizoma coptidis four flavour is crushed into fine powder; The bezoar porphyrization, and the running-in powder, sieving, blending. Per 100 g powder refining honey made big honey pill, 100 ~ 120 g for a quick.
【 characteristics 】 this product is a reddish brown to brown big honey pill; Specific and sweet, slightly astringent and bitter taste.
[identify] (1) take this product, buy a microscope: gelatinized starch grain mass almost colorless (turmeric). Kind of PiShi fine
Yellow or pale brown, broken, more complete long polygon, rectangle or irregular shape, wall thickness, has a big round pit, cellular palm red (gardenia). Bast fiber light yellow, fusiform, wall thickness, hole groove (scutellaria baicalensis). Fiber bundle of bright yellow, slightly thick wall, pit (coptis chinensis) obviously. Irregular tiny particles is dark brown, shiny, margin dark (cinnabar).
(2) take this product for 3 g, add water right amount, grind, repeatedly wash suspended matter, can get a little red precipitate. Precipitation, add 1 ml of hydrochloric acid and a small amount of copper, heat to boil, copper changed from yellow to white.
(3) take this product for 3 g, cut up, add diatomite 0.6 g, grind, add 10 ml of chloroform, glacial acetic acid 0.5 ml, heating reflux 30 minutes, put the cold, filtration, the filtrate to dry, residual ethanol 2 ml to dissolve, filtration, the filtrate greatly as the solution. The bile acid reference substance, add ethanol made from each 1 ml solution containing 1 mg, as a reference substance solution. According to thin layer chromatography (TLC) (0502) the general principles of the test, each 10 (including l learned these two solutions, each point in the same silica G thin layer plate, with n-hexane - ethyl acetate - methanol - acetic acid (6:32:1:1) as an agent,, remove and dry spray phosphomolybdic acid at 10% ethanol solution, heating at 110 ℃ for 10 minutes. In the chromatogram of the test, with the reference substance chromatography corresponding position, the same color spots.
(4) take this product for 3 g, cut up, add diatomite 0.5 g, grind, methanol 20 ml, heating reflux for 1 hour, put the cold, filtration, the filtrate greatly as the solution. Another take baicalin reference substance, and made each 1 ml contains 1 mg of methanol solution, as a reference substance solution. According to thin layer chromatography (TLC) (0502) general test, 5 (including l learned these two solutions, each point in the same containing 4% of sodium carboxymethyl cellulose sodium acetate solution as adhesive of silica G thin layer plate, in ethyl acetate - butyl ketone - formic acid and water (5:3:1:1) as an agent, and taken out, dry spray with ferric chloride 2% ethanol solution. In the chromatogram of the test, with the reference substance chromatography corresponding position, the same color spots.
(5) take this product for 3 g, and ether 15 ml, grinding, abandon to ether liquid, liquid to wash the ether, and ethyl acetate 30 m1, heating reflux for 1 hour, put the cold, filtration, the filtrate zhenggan residue plus 3 ml methanol dissolved, filtration, the filtrate greatly as the solution. Another gardenoside reference substance, and made each 1 ml contains 1 mg of methanol solution, as a reference substance solution. According to thin layer chromatography (TLC) (0502) general test, 5 (including l learned these two solutions, each point in the same silica G thin layer plate, with ethyl acetate - acetone - formic acid - water (10; 7:2:0. 5) as developing agent, and taken out, dry spray with 10% ethanol solution of sulfuric acid heating at 105 ℃ for 10 minutes. In the chromatogram of the test, with the reference substance chromatography corresponding position, the same color spots.
(6) in [on] content of rhizoma coptidis under as the product of test sample solution solution. Take 50 mg of rhizoma coptidis contrast medicinal material, add 10 ml of methanol, heating reflux 15 minutes, filtration, the filtrate zhenggan residue with methanol 1 ml to dissolve, as a control medicine solution. Another take berberine hydrochloric acid reference substance, and made each 1 ml contains 0.5 mg of methanol solution, as a reference substance solution. According to thin layer chromatography (TLC) (0502) the general principles of the test, from the above three kinds of solution (including 2 l, each point in the same silica G thin layer plate, with toluene, ethyl acetate, isopropyl alcohol - methanol - concentrated ammonia solution (12:6:3:3:1) as developing agent, under ammonia vapor saturation, remove and dry, can be examined under a uv lamp (365 nm). In the chromatogram of the test, to the chromatographic and reference substance chromatography corresponding position, shows the same yellow fluorescence spots.
Check hyodeoxycholic acid 】 take this product, cut up, 0.6 g, join the amount of diatomite, fine, add 50 ml methanol, heating reflux 3 hours, filtration, the filtrate zhenggan residue add 5 ml of ethanol ultrasonic dissolving, centrifugal, take that as a solution of the supernatant fluid. Another hyodeoxycholic acid reference substance, adding ethanol made from each 1 ml solution containing 0.5 mg, as a reference substance solution. According to thin layer chromatography (TLC) (0502) general test, 5 mu l learned these two solutions, each point in the same silica G thin layer plate, with cyclohexane - ethyl acetate - 36% acetic acid - methanol (20:25:2:3) the upper solution for developing agent, 2 times, remove and dry spray with 10% ethanol solution of sulfuric acid in the 105 ℃ heating to the spot color is clear, respectively under the sunlight and ultraviolet light (365 nm). In the chromatogram of the test, with the reference substance chromatography corresponding position, may not be the same color spots and fluorescence spots.
Free bilirubin According to high performance liquid chromatography determination of the general principles of the (0512) (dark) operation.
Chromatographic conditions with system suitability test under [on] content of bilirubin.
The preparation of the reference substance solution the right amount of bilirubin reference substance, precision said, and made each 1 ml methylene chloride solution containing 6.5 mu g, quick.
The preparation of test sample solution: take this product under a weight difference, cut up, take about 2 g, precision said, precision to join a moderate amount of anhydrous calcium carbonate (according to the sample with 1 ~ 2 times the amount of moisture content), fully porphyrization after blending, the right amount of powder (equivalent to taking 413 mg) of this product, the precise said, with a plug in the conical flask, precision in methylene chloride 20 ml, plug, said weight, vortex to thoroughly incorporated, ice bath ultrasonic processing (power 500 w, 53 KHZ frequency) 30 minutes, and then according to weight, lose weight reduction with methylene chloride, shake well, centrifugal (rotating speed is 4000 RPM), take dichloromethane solution, filtration, take the filtrate, quick.
Measurement precision respectively from the reference substance solution and 5 mu l of test sample solution, injection liquid chromatograph, determination, quick.
In the chromatogram of the test, with the reference substance chromatographic peak retention time corresponding to the position, there should be less than the chromatographic peak
According to the chromatographic peak, peak or not.
Other should conform to the provisions of the pill under the general principles of the (0108).
Bilirubin content determination 】 【 as high performance liquid chromatography determination of the general principles of the (0512) (dark) operation.
The chromatographic conditions and system suitability test Octadecyl silane bonded silica gel as filling agent; With acetonitrile - 1% glacial acetic acid (95:5) as mobile phase; Detection wavelength of 450 nm. Theoretical plate number calculated on bilirubin peak should be not less than 3000.
The preparation of the reference substance solution the right amount of bilirubin reference substance, precision said, adding methylene chloride (including each 1 ml contains 10 g solution, quick.
The preparation of test sample solution take weight difference on our product, cut up, about 0.5 g, precision said, precision to join the diatomite in moderation, fully porphyrization after blending, the right amount of powder (the equivalent of this product is about 0.1 g), precision said, with a plug in the conical flask, adding 10% oxalic acid solution (containing 0.15% cetyl trimethyl ammonium chloride) 4 ml, plug, vortex to thoroughly incorporated, precision water saturation 20 ml methylene chloride, plug, said weight, vortex to thoroughly incorporated, ultrasonic processing (power 500 w, 53 KHZ frequency) 30 minutes, put the cold, again according to weight, water saturated methylene chloride make up the weight loss reduction, shake well, centrifugal (rotating speed is 4000 RPM), take dichloromethane solution, filtration, take the filtrate, quick.
Measurement precision respectively from the reference substance solution and 5 mu l of test sample solution, injection liquid chromatograph, determination, quick.
This product per pill containing bezoar or in vitro cultivation bezoar in bilirubin (C33H36N4O6), [specification] (1) shall not be less than 2.0 mg, (2)] [specifications shall not be less than 4.0 mg.
Vermilion: take this product under a weight difference, shear, blending, take about 5 g, precision said, 250 ml kjeldahl flask, plus 30 ml sulphuric acid and potassium nitrate 8 g, initiate to almost colorless solution heat, cold, into 250 m1 in the conical flask, 50 ml by several times with water wash flask, lotion into solution, 1% potassium permanganate solution to pink and not disappear within two minutes, then add 2% ferrous sulfate solution to red disappeared, with ammonium ferric sulfate indicating liquid 2 ml, with ammonium thiocyanate titration fluid (0.1 mol/L) titration. Each 1 ml ammonium thiocyanate titration fluid (0.1 mol/L) is equivalent to 11.63 mg of mercuric sulfide (HgS).
This product per pill containing cinnabar in mercuric sulfide (HgS), (1) should be 69 ~ 90 mg; (2) should be 138 ~ 180 mg.
The general principles of the coptis chinensis as high performance liquid chromatography (0512).
The chromatographic conditions and system suitability test Octadecyl silane bonded silica gel as filling agent; With acetonitrile - 0.05 mol/L of potassium dihydrogen phosphate solution (50:50) (0.4 g per 100 ml adding sodium dodecyl sulfate, to adjust pH value of 4.0) phosphate as mobile phase; Detection wavelength of 345 nm. Theoretical plate number calculated on berberine hydrochloride peak should be not less than 5000.
The preparation of the reference substance solution the right amount of berberine hydrochloride reference substance, precision said, adding methanol each 1 ml contains 80 (including g solution, quick.
The preparation of test sample solution take weight difference on our product, cut up, blending, about 0.3 g, precision said, with a plug in the conical flask, precision in hydrochloric acid - methanol (1:100) mixture 25 ml, said weight, 85 ℃ water bath heating reflux in 40 minutes, put the cold, again according to weight, hydrochloric acid - methanol (1:100) mixture make up the weight loss reduction, shake well, centrifugal, supernatant fluid filtration, take the filtrate, quick.
Measurement precision respectively from the reference substance solution and 5 mu l of test sample solution, injection liquid chromatograph, determination, quick.
This product per pill containing rhizoma coptidis with berberine hydrochloride (C20H17NO4 · HCl) meter, pellet shall not be less than 7.5 mg; Shall not be less than 15.0 mg.
【 functions and indications 】 qingrejiedu, of nerves. Used for heat into the pericardium, dynamic wind heat syndrome, disease see hot fidgety, god faint delirious speech and children with febrile convulsion.
[usage and dosage 】 oral. A 2 pills/specifications (1) or a 1 pill/specifications (2), 2 ~ 3 times a day.
【 note 】 if pregnant.
【 specification 】 (1) each pill weighs 1.5 g per pill (2) 3 g
【 storage 】 sealed.
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