2 Biyantong Spray (Biyantong Drops) Pharmacopoeia Standard 2. 1 Name Biyantong Spray (Biyantong Drops)
Biyan Tongpenwuji
2.2 Prescription of ephedrine hydrochloride 5g, baicalin 20g, honeysuckle 300g, magnolia oil 2ml, borneol1g..
2.3 Take the above five ingredients, add appropriate amount of water to baicalin, stir evenly, add appropriate amount of 40% sodium hydroxide solution to dissolve, adjust the pH value to 6.5 ~ 7.5 with dilute hydrochloric acid, decoct honeysuckle with water twice, filter, combine filtrates, concentrate to fluid extract with relative density of about 65438 0.05 (50℃), cool, and add 20%. Adjust the pH value to 3.5 ~ 4.0 with 50% sulfuric acid solution, stir evenly, filter, adjust the pH value of the filtrate to 6.5 ~ 7.0 with 40% sodium hydroxide solution, seal, refrigerate for 2 ~ 3 days, filter, recover ethanol from the filtrate, concentrate to about 25ml, add water, stir evenly, treat with activated carbon, and filter. Ephedrine hydrochloride is dissolved in water for later use. Dissolve Borneolum Syntheticum and Flos Magnoliae Oil in ethanol, then add 2 1g polysorbate 80, stir well, add the above liquid medicine, then add 0.8g sodium bisulfite and 10g benzyl alcohol, mix well, add water to nearly the total amount, stir well, adjust the pH value to 6.0-7.0, filter and add water to 1000ml.
2.4 Characteristics This product is a spray, and the liquid medicine is a yellow-brown to brown clear liquid.
2.5 Identification (1) Take 30ml of this product, add 1.2g of calcium hydroxide, stir 10min, centrifuge, take the supernatant, add 30ml of petroleum ether (30 ~ 60℃), shake and extract, separate petroleum ether solution, and add 6mol/L hydrochloric acid solution/kloc-. In addition, Flos Magnoliae 1g was taken as the control medicinal material and tested according to the method of volatile oil determination (Appendix X D A of Pharmacopoeia 20 10). Add 2ml of ethyl acetate into the measuring cylinder, heat it to boiling, keep it slightly boiling for 65438+/-0h, then divide the ethyl acetate solution, add 0.2g of anhydrous sodium sulfate, stir it evenly, and centrifuge it as a control medicinal solution. Then, take the borneol reference substance and add petroleum ether (30 ~ 60℃) to make a solution containing 3mg per 1ml as the reference substance solution. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia I, 20 10), the above-mentioned test solution 10μl, reference medicinal solution 5 ~ 6μ l and reference medicinal solution 5 ~ 6μ l were respectively absorbed and spotted on the same silica gel G thin-layer plate to make strips. In the chromatogram of the test sample, petroleum ether (30 ~ 60℃)- ethyl acetate (8: 1) is used, and there are more than two spots with the same color at the positions corresponding to the chromatogram of the control medicinal materials; At the position corresponding to the chromatogram of the reference substance, spots with the same color are displayed.
(2) Take this product 10ml, add 20ml of ether, gently shake and extract, separate the aqueous solution, evaporate to dryness, add 3ml of methanol to dissolve the residue, filter, and take the filtrate as the test solution. In addition, 65438 0 g of Flos Lonicerae was taken as the control medicinal material, 5ml of methanol was added, and ultrasonic treatment was carried out for 65438±00min, 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), 2 ~ 5 μ l of each of the above three solutions was absorbed, spotted on the same silica gel G thin-layer plate, and the upper solution of butyl acetate-formic acid-water (7: 2.5: 2.5) was used as the developing agent, developed, taken out, dried and placed under an ultraviolet lamp (365nm). In the chromatogram of the test sample, fluorescent spots with the same color appear at the positions corresponding to the chromatograms of the reference medicinal materials and the reference substance.
2.6 Check that the pH value of 2.6. 1 should be 4.5 ~ 7.0 (Appendix VII g of Pharmacopoeia 20 10).
2.6.2 Spray test Take this product and check it according to the spray test (Appendix I Z of Pharmacopoeia 20 10). The average spray quantity of each bottle should be 0.063~0.095g
2.6.3 Others shall comply with the relevant provisions under nasal preparations (Appendix ix of Pharmacopoeia I, 20 10).
2.7 Content determination 2.7. The content of1baicalin was determined by high performance liquid chromatography (Appendix ⅵ d of Pharmacopoeia I, 20 10 edition).
2.7. 1. 1 chromatographic conditions and system applicability test, with octadecylsilane bonded silica gel as filler; Using methanol -0.2% phosphoric acid solution (52∶48) as mobile phase; The detection wavelength is 280 nm. According to the peak of Scutellaria baicalensis Georgi, the theoretical plate number should be no less than 2000.
2.7. 1.2 Preparation of reference solution Take a proper amount of Scutellaria baicalensis Georgi reference, weigh it accurately, and add dilute ethanol to make a solution containing 0. 1mg per 1ml.
2.7. 1.3 preparation of test solution accurately weigh 0.5ml of this product, put it in a bottle with 100ml, add 2 drops of 6mol/L hydrochloric acid solution, heat it in warm water for 3 minutes, shake it evenly, add dilute ethanol to the scale, shake it evenly, filter it, and take a continuous filtrate.
2.7. 1.4 Determination method Accurately suck the control solution and the test solution 10μl respectively, inject them into the liquid chromatograph, and determine.
Every 1ml of this product contains baicalin (C2 18O 1 1) which should be 85.0% ~ 1 15.0% of the labeled amount.
2.7.2 the content of ephedrine hydrochloride was determined by high performance liquid chromatography (appendix ⅵ D of pharmacopoeia I, 20 10 edition).
2.7.2. 1 chromatographic conditions and system applicability test: octadecylsilane bonded silica gel is used as filler; Methanol -0.009mol/L sodium heptane sulfonate solution and 0.05mol/L potassium dihydrogen phosphate solution (adjusted to pH 3.0 with phosphoric acid) (40: 60), mobile phase: 1% triethylamine; The detection wavelength is 2 13 nm. Calculated by ephedrine hydrochloride peak, the theoretical plate number should be no less than 1000.
Preparation of 2.7.2.2 Reference Solution Take an appropriate amount of ephedrine hydrochloride reference substance, weigh it accurately, and add the mobile phase to make a solution containing 0.65438±0mg per 65438±0ml.
Preparation of 2.7.2.3 test solution Accurately measure 65438±0ml of this product, put it in a 25ml volumetric flask, add about 20 ml of 0.3% calcium hydroxide solution (shake well before use), heat it with warm water for 5 5minutes, cool it to room temperature, ultrasonically treat it (power 300W, frequency 40 kHz) 40k Hz)65438±0min, add 0.3% calcium hydroxide solution to the scale, and shake well to get the product. Add 3 drops of 6mol/L hydrochloric acid solution, shake well, evaporate to dryness, dissolve the residue with a proper amount of mobile phase, transfer to a 10ml volumetric flask, add the mobile phase to the scale, shake well, filter and take the filtrate.
2.7.2.4 method accurately absorbs 65438 00μ l of control solution and test solution respectively, and injects them into liquid chromatograph for determination.
Ephedrine hydrochloride (C 10H 15no HCl) in this product should be 85.0% ~ 1 15.0% of the labeled amount.
2.8 Indications: expelling wind and clearing heat, dispersing lung qi and dredging orifices. Used for nasal congestion, clear or turbid nasal discharge, fever and headache caused by wind-heat accumulation in lung; Acute and chronic rhinitis with the above syndrome.
2.9 Administration and dosage: spray into nasal cavity, once 1 ~ 2 capsules; 2 ~ 4 times a day. 1 month is a course of treatment.
2. 10 specification (1) per bottle 10ml? (2) Each bottle contains 15ml (each bottle contains 20mg of baicalin and 5mg of ephedrine hydrochloride).
2. 1 1 Storage is light-proof and sealed.
2. 12 attachment: Flos Magnoliae Oil This product is Flos Magnoliae Pamp. And magnolia. Magnoliaceae. Or volatile oil extracted from dried flower buds of Magnolia grandiflora by steam distillation.
2. 12. 1 properties this product is a light yellow to yellow clear liquid; It has a special fragrance of magnolia flowers and a spicy taste.
2. 12.2 Identification Take 0.05ml of this product, add 1 ml petroleum ether (60 ~ 90℃) and dissolve it as the test solution. In addition,1g. Taking Flos Magnoliae as control. Add 2ml petroleum ether (60 ~ 90℃) into the measuring cylinder according to the method for determination of volatile oil (Appendix X D A of Pharmacopoeia 20 10), and heat it to boiling, keeping it slightly boiling1h. Then, petroleum ether solution was separated, 0.2g anhydrous sodium sulfate was added, stirred evenly, and dehydrated. According to the test of thin-layer chromatography (Appendix ⅵ b of Pharmacopoeia I, 20 10), respectively absorb the above two solutions 1μl on the same silica gel G thin-layer plate, and use petroleum ether (30 ~ 60℃)- ethyl acetate (80: 7) as developing agent, unfold, take out and dry. Spray 2% vanillin with 10% sulfuric acid ethanol solution, and heat at 105℃ until the spots are clear. In the chromatogram of the test sample, the spots with the same color appear at the positions corresponding to the chromatogram of the control medicinal materials.
2. The relative density of12.3 cha 2. 12.3.1should be 0.870 ~ 0.940 (Appendix VII A of Pharmacopoeia 20 10).
2. 12.3.2 The refractive index should be 1.457 ~ 1.487 (Appendix VII of Pharmacopoeia 20 10).
2. 12.4 Store in the dark, sealed and placed in the shade.
Version 2. 13