柴葛退热散超微粉碎工艺优化

Optimization of Ultrafine Pulverization Technology in Chaige Tuire Powder

目的:优化柴葛退热散超微粉碎工艺;比较超微粉和普通细粉中有效成分的含量和显微特征。方法:以柴葛退热散中3种有效成分(葛根素、甘草苷和黄芩苷)的含量以及粉末d(0.5)为主要指标,以堆密度、休止角及显微特征为参考指标,设计正交试验对超微粉碎工艺中粉末的初始粒径、水分及粉碎频率进行优化。比较超微粉与普通细粉(过65/80目筛)中3种有效成分的含量及显微镜下草酸钙针晶的观察结果。结果:超微粉优化工艺为选择初始粒径为过65目筛、水分为2.5%的药材粉末在粉碎频率为60 Hz下粉碎;验证试验中3份超微粉样品的d(0.5)平均值为31.5μm(RSD=0.45%,n=3),其中葛根素、甘草苷和黄芩苷的含量分别为0.232、0.212、8.962 mg/g(RSD分别为1.31%、1.62%、0.89%,n=3),比普通细粉中3种有效成分含量(0.158、0.160、6.140mg/g)约高30%~40%。超微粉中未见或仅少量可见普通细粉中常见的成束草酸钙针晶。结论:优化的超微粉碎工艺稳定、可行;柴葛退热散超微粉中3种有效成分的含量高于普通粉中含量,且因草酸钙针晶的减少有可能减少其临床不良反应。

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.