RESUMO
OBJECTIVE:To optimize the ultrafine pulverization technology in Chaige tuire powder;to compare the content and microcharacteristics between ultrafine powder and ordinary powder. METHODS:Using contents of 3 active ingredients(puera-rin,glycyrrhizin and baicalin)and powder d(0.5)as main indexes,bulk density,angle of repose and microcharacteristic as refer-ence indexes,orthogonal test was designed to optimize the initial particle size,moisture and pulverized frequency in ultrafine pul-verization technology. Contents of 3 active ingredients of ultrafine powder and ordinary powder(over 65/80 mesh sieve)and obser-vation results of calcium oxalate crystal under microscope were compared. RESULTS:The optimized technology was as follow as over 65 mesh sieve,moisture of 2.5%preliminary powder in 60 Hz of frequency for pulverization. In verification test,d(0.5)aver-age value of 3 ultrafine powder samples was 31.5 μm(RSD=0.45%,n=3);contents of puerarin,glycyrrhizin and baicalin were 0.232 mg/g(RSD=1.31%,n=3),0.212 mg/g(RSD=1.62%,n=3),8.962 mg/g(RSD=0.89%,n=3),respectively,which were increased about 30%-40% than in ordinary powder(0.158,0.15669,6.140 mg/g). There were no or little bundles of calci-um oxalate crystal that is common in ordinary powder. CONCLUSIONS:Optimized ultrafine pulverization technology is stable and feasible;contents of 3 active ingredients in Chaige tuire ultrafine powder are higher and calcium oxalate crystal are litter than ordi-nary powder,which possibly reduces the adverse reactions in clinical application.
RESUMO
Objective To establish ultra-high performance liquid chromatography-evaporative light scattering detector (UPLC-ELSD) method to determine the content of astragaloside in Guiqi Yiqi Yangxue Mixture and optimize the best water decoction process of the mixture.Methods The UPLC-ELSD conditions to determine the content of astragaloside in the mixture were as follow.The method was carried out on a Waters Acquity UPLC BEH C18 column (2.1 mm ×50 mm,1.7 μm) by using acetonitrile-water (35∶65) as mobile phase, and the flow rate was 0.3 mL/min and the column temperature 30℃.The parameter of ELSD:the drift tube temperature was set at 60℃, and the gas flow rate of N2 2.0 L/min.The content of paeoniflorin in the mixture was detected by previously established HPLC method.The orthogonal test was designed to optimize the water decoction process of the amount of water (A), decoction time (B) and decoction times (C), and the extract yield and the contents of astragaloside and paeoniflorin were evaluated as the comprehensive markers for the purpose.Results The UPLC-ELSD determination of astragaloside had a good linear relationship (r =0.9999), its mean recovery was 103.0%, and it had a good precision, specificity and repeatability.The orthogonal experimental results showed that decoction times (C) >the amount of water (A) >decoction time (B) were major factors affecting the decoction process in order and the ANOVA result showed that decoction times has significant effect on the decoction process (P<0.05).The optimal process of Guiqi Yiqi Yangxue Mixture was adding eight-fold water each time to decoct twice for 1.5 h totally.Conclusion This optimized water decoction process is feasible and stable, and suitable for industrialized production.