Study On The Preparation Process And Quality Standard Of DIAOLIU Granules

Objective:Study on the extraction process and forming process of the withering granules,and carry out research on the quality standards of the withering granules,laying a foundation for the development and production of withering granules.Methods:1.Study on extraction technology: comprehensive analysis was conducted on the effective components of various herbs,and the alcohol extraction technology of fructus ligustrum,fructus psoralea,turmeric,and radix lithospermum was investigated.The single factor method combined with Box-Behnken response surface method was used to determine the optimal extraction conditions by taking the content of privet glycoside,the content of psoralen and the yield of dry paste as the comprehensive indicators,and investigating the ethanol concentration,alcohol dosage,extraction time and extraction times;Then the water extraction technology of astragalus and seaweed was studied.Single factor combined with Box-Behnken response surface method,astragaloside Ⅳ content,seaweed polysaccharide content and dry paste yield were used as comprehensive indicators to investigate the amount of water added,frying time,frying times,to determine the optimal water extraction process conditions.2.Research on molding process: take particle molding rate,hygroscopicity and fluidity as indicators to screen the best molding process.3.Study on quality standards: the quality standards of granules were established from three aspects:qualitative identification,content determination and relevant examination.TLC method was used to identify the components of shikao,turmeric,fructus psoraleae and other traditional Chinese medicines in DIAOLIU granules.HPLC method was used to determine the content of privet glycoside and astragaloside in granules,and to conduct methodological investigation.In addition,limited testing was conducted for the toxic medicinal materials strychnine and centipede in granules.Results: The best alcohol extraction process of withered tumor granules is 8 times the amount of 50% ethanolreflux extraction 2 times,each 90 minutes;The best water extraction process is to soak in10 times the amount of water for 120 minutes,extract twice,and the extraction time is 60minutes;The best molding process is dry paste powder and(dextrin + sucrose)mixed auxiliary materials in a ratio of 2:1 to mix evenly,with 95% ethanol as wetting agent,at60℃for drying,take out,the whole grain;A TLC method was established for the identification of rhizoma cyperi,turmeric and psoralea psoralea in the DIAOLIU granules.HPLC-ELSD method was used to determine the content of astragaloside a in granules.The chromatographic conditions were as follows: mobile phase:acetonitrile-water(32:68).Flow rate: 1mL/min;Injection volume: 20 μl;Column temperature: 30℃;ELSD drift tube temperature: 40℃;Carrier gas: high purity nitrogen,under the condition of astragaloside a good methodological investigation,can be used to establish astragalus quality standards;HPLC method was used to limit the content of brucine and strychnine.The chromatographic conditions were: acetonitrile-0.01% sodium heptane sulfonate and 0.02% potassium dihydrogen phosphate(adjust pH to 2.7 with 10%phosphoric acid)(30:70),the detection wavelength is 260 nm,the column temperature is30℃,the flow rate is 1mL / min;this method detects that the content of strychnine is0.0846 mg/g,which has a concentration range of 0.0024~0.0120 mg/mL good linear relationship;The granule related inspections are in compliance with the requirements of the Chinese Pharmacopoeia(2015 edition).Conclusion: The production process of DIAOLIU granules is reasonable and feasible;the quality standards formulated are accurate and reproducible,which can effectively control the quality of the preparations.