2. The pharmacopoeia standard of Lianhua Qingwen Granules 2. 1 is called Lianhua Qingwen Granules.
Lianhua Qingwen Granule
2.2 prescription forsythia suspensa 170g, honeysuckle 170g, fried ephedra 57g, fried bitter almond 57g, gypsum 170g, isatis root 170g, cyrtomium rhizome 170g, houttuynia cordata 170g.
2.3 Distilling the thirteen medicinal materials with water to extract volatile oil, collecting the volatile oil, and filtering the water extract for later use; Fructus Forsythiae, Herba Ephedrae preparata, Herba Houttuyniae and Radix et Rhizoma Rhei were heated and refluxed twice with 70% ethanol, the first time was 2 hours, and the second time was 65438 0.5 hours. Filtering, mixing extractive solutions, and recovering ethanol for later use. Boil Flos Lonicerae, Gypsum Fibrosum, Radix Isatidis, Dryopteris Dryopteris, Radix Glycyrrhizae, and Radix Rhodiolae in water, add parched bitter almond, decoct twice, the first time is 65,438 0.5 hours, and the second time is 65,438 0.0 hours, filter the decoctions, combine the filtrates, add the aqueous solution extracted from Pogostemon cablin, and concentrate to the relative density of 65,438 0.65,438 0. Adding ethanol to make the alcohol content reach 70%, refrigerating at 4℃ for 24 hours, filtering, recovering ethanol from the filtrate, mixing with the spare ethanol extracts of Fructus Forsythiae and other four medicines, concentrating to a relative density of 65,438+0.25 ~ 65,438+0.35 (60℃), adding sugar powder and dextrin, mixing, granulating, drying, sieving and so on.
2.4 Characteristics This product is brownish yellow to brownish brown granules; The gas is slightly fragrant and the taste is slightly bitter.
2.5 Identification (1) Take 6g of this product, crush it, add 10ml methanol, perform ultrasonic treatment for10min, filter it, evaporate the filtrate, dissolve the residue with 10ml water, transfer it to a separating funnel, and shake and extract it with ether twice, each time. In addition, 0.5g of Flos Lonicerae was taken as the control medicinal material, 8ml of methanol was added, and ultrasonic treatment was performed for 10 minute, and the filtrate was taken as the control medicinal material solution. Then take chlorogenic acid reference substance, add methanol to make a solution containing 65438±0mg per 65438±0ml as reference substance solution. According to the test of thin-layer chromatography (appendix ⅵ b of Pharmacopoeia I, 20 10), absorb 4 ~ 8 μ l of the above three solutions, spot them on the same silica gel G thin-layer plate, and use the upper liquid of butyl acetate-formic acid-water (14: 5: 5) as the developing agent, unfold, take them out and place them under ultraviolet light (365nm). In the chromatogram of the test sample, at least two fluorescent spots with the same color appear at the position corresponding to the chromatogram of the control medicinal material; At the position corresponding to the chromatogram of the reference substance, fluorescent spots with the same color are displayed.
(2) Take the test solution under [Identification] (1) as the test solution. In addition, 65438 0 g of Glycyrrhiza uralensis Fisch was taken, 8ml of methanol was added, and ultrasound was performed for 65438 00 minutes, and the filtrate was used as the control medicinal material solution. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia Part I, 20 10), 4 ~ 8 μ l of the test solution and 4μl of the control medicinal solution were respectively spotted on the same silica gel G thin-layer plate, and the lower solution of chloroform-methanol-water (13: 6: 2) 10℃ was used as the developing agent. In the chromatogram of the test sample, the main spots with the same color are displayed at the corresponding positions of the chromatogram of the control medicinal materials.
(3) Take this product 12g, grind it, add ethanol 10ml, ultrasonic10min, let it stand, and take the supernatant as the test solution. In addition, 0.5g of rhubarb was taken as the control medicinal material, and 3ml of methanol was added to prepare the control medicinal material solution in the same way. Then take 0.5g of Houttuynia cordata Thunb, add 5ml of methanol, perform ultrasonic treatment for 20min, filter, and take the filtrate as the control medicinal material solution. According to the test of thin-layer chromatography (appendix ⅵ b of Pharmacopoeia I, 20 10), absorb 4 ~ 8 μ l of each of the above three solutions, spot them on the same silica gel G thin-layer plate, and use cyclohexane-ethyl acetate-formic acid (4: 1: 0. 1) as the developing agent, unfold, take them out and place them in ultraviolet light. At least two identical orange-yellow fluorescent spots appear in the chromatogram of the test sample at the position corresponding to the chromatogram of the rhubarb control medicinal material; At the position corresponding to the chromatogram of Houttuynia cordata Thunb, at least three fluorescent main spots with the same color are displayed.
(4) Take the test solution under [Identification] (3) as the test solution. Another ephedrine hydrochloride reference substance was added with methanol to prepare a solution containing 1 mg per 1 ml as the reference substance solution. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia Part I, 20 10), on the same silica gel G thin-layer plate, 5 ~ 10 μ l of test solution and 5μl of reference solution were absorbed respectively, and chloroform-methanol-concentrated ammonia solution (20: 4: 0.5) was used as developing agent, and then unfolded, taken out and dried. In the chromatogram of the test sample, spots with the same color appear in the position corresponding to the chromatogram of the control sample.
(5) Take 6g of this product, grind it, add 5ml of petroleum ether (60 ~ 90℃), shake it evenly for 2min, filter it, and take the filtrate as the test solution. Another menthol reference substance was added with methanol to prepare a solution containing 0.5 mg per kloc-0/ml as the reference substance solution. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia Part I, 20 10), take 4 ~ 8 μ l of test solution and 4μl of reference solution, respectively, and spot them on the same silica gel G thin-layer plate, using cyclohexane-ethyl acetate-formic acid (4: 1: 0. 1) as the developing agent, and unfold them. In the chromatogram of the test sample, spots with the same color appear in the position corresponding to the chromatogram of the control sample.
2.6 Check 2.6. 1 Honeysuckle Take 6g of this product, crush it, add 20ml of methanol, ultrasonic wave for 65438±05min, filter it, evaporate the filtrate, add 20ml of water to dissolve the residue, shake and extract it with water-saturated n-butanol twice, 30ml each time, combine the n-butanol solutions, wash them twice with ammonia test solution, and evaporate the n-butanol solution. Another reference substance, Lonicera macranthoides saponin B, was added with methanol to make a solution containing 1ml as the reference substance solution. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia I, 20 10), 4μl of test solution and 2μl of reference solution were respectively absorbed on the same silica gel G thin-layer plate, and chloroform-methanol-water (6: 4: 1) was used as the developing agent, and then developed, taken out, dried and sprayed with 65438+. In the chromatogram of the test sample, the spots with the same color shall not be displayed in the position corresponding to the chromatogram of the reference sample.
2.6.2 Others shall comply with the relevant provisions under granules (Appendix I C of Pharmacopoeia I, 20 10).
2.7 the content was determined by high performance liquid chromatography (appendix ⅵ D of pharmacopoeia I, 20 10).
2.7. 1 chromatographic conditions and system applicability test, using octadecylsilane bonded silica gel as filler; Acetonitrile -0. 1% phosphoric acid solution (22∶78) was used as the mobile phase. The detection wavelength is 205 nm. The theoretical plate number should be not less than 3500 calculated by Fossettin peak.
2.7.2 Preparation of reference solution Take a proper amount of phillyrin reference substance, weigh it accurately, and add 50% methanol to make a solution containing 4μg per 1ml.
2.7.3 Preparation of test solution Take the products with different volumes, mix them evenly, take an appropriate amount, grind them, take 2g, weigh them accurately, put them in a conical flask with a stopper, add 25ml of methanol accurately, plug them, weigh them, perform ultrasonic treatment (power 250W, frequency 40kHz) for 30min, let them cool, weigh them again, and make up the weight loss with methanol. Adding neutral alumina column (100 ~ 200 mesh, 3g, inner diameter 1cm), eluting with water, collecting eluate in 25ml volumetric flask, weighing, shaking, filtering, and collecting filtrate.
2.7.4 Determination Method Accurately absorb 10μl of control solution and test solution, inject them into high performance liquid chromatograph, and determine.
Each bag of this product contains Fructus Forsythiae (C27H34O 1 1), which shall not be less than 0.69mg.
2.8 Function: clearing away pestilence and detoxicating, dispersing lung and clearing heat. Can be used for treating lung influenza caused by heat toxin. Symptoms are fever, aversion to cold, muscle aches, nasal congestion and runny nose, cough, headache, dry throat and sore throat, red tongue, yellow or greasy fur.
2.9 Usage and dosage of Lianhua Qingwen Granules are taken orally. 6g once, 3 times a day.
2. 10 specification 6g per bag.
2. 1 1 Store in a cool place and keep it sealed.
Version 2. 12