摘要
目的:建立测定妇科再造丸体外溶出度的方法。方法:采用高效液相色谱法测定制剂中黄芩苷和橙皮苷的含量,色谱柱为Wonda Sil-C18,流动相为0.2%甲酸溶液-乙腈(梯度洗脱),流速为1.0 m L/min,检测波长为280 nm,柱温为30℃,进样量为10μL;采用桨法测定制剂的累积溶出度,溶出介质为磷酸盐缓冲液(p H 6.8),转速为100 r/min,温度为(37±0.5)℃,取样量为2 m L。结果:黄芩苷和橙皮苷检测质量浓度线性范围分别为6.936~23.12μg/m L(r=0.999 8)、0.620~3.10μg/m L(r=0.999 0);定量限分别为4.624、0.620μg/m L,检测限分别为2.312、0.155μg/m L;精密度、稳定性、重复性试验的RSD均小于2%;加样回收率分别为95.28%~99.22%(RSD=0.97%,n=9)、96.10%~99.84%(RSD=1.98%,n=9)。样品中黄芩苷和橙皮苷10 h时的平均累积溶出度分别为(97.10±0.09)%、(78.50±0.08)%;溶出63.2%所需时间(TD)分别为(1.88±0.12)、(3.26±0.10)h,溶出50%所需时间(T50)分别为(0.88±0.09)、(1.67±0.14)h。结论:该方法操作简便、准确,可用于妇科再造丸的体外溶出度测定。
OBJECTIVE:To establish a method for the determination of in vitro dissolution of Fuke zaizao pills.METHODS:HPLC method was adopted to determine the contents of baicalin and hesperidin in preparation.The determination was performed on WondaSil-C18 column with mobile phase consisted of 0.2%formic acid-acetonitrile(gradient elution)at the flow rate of 1.0 mL/min.The detection wavelength was set at 280 nm,and column temperature was 30℃.The sample size was 10μL.The dissolution of the preparation was determined by paddle method using phosphate buffer solution(pH 6.8)as dissolution medium with rotate speed of 100 r/min,temperature was(37±0.5)℃,sample size was 2 mL.RESULTS:The linear range of baicalin and hesperidin were 6.936-23.12μg/mL(r=0.999 8)and 0.620-3.10μg/mL(r=0.999 0),respectively.Limits of quantitation were 4.624,0.620μg/mL,limits of detection were 2.312,0.155μg/mL,respectively.RSDs of precision,stability and repeatability tests were all lower than 2%;the recoveries were 95.28%-99.22%(RSD=0.97%,n=9)and 96.10%-99.84%(RSD=1.98%,n=9),respectively.The accumulative dissolution rates of baicalin and hesperidin in sample were(97.10±0.09)%and(78.50±0.08)%at 10 h,respectively.TD were(1.88±0.12)、(3.26±0.10)h,T50 were(0.88±0.09)、(1.67±0.14)h,respectively.CONCLUSIONS:The method is simple and accurate,and can be used for the determination of in vitro dissolution of Fuke zaizao pills.
作者
郑晓霞
徐剑
田洪星
胡蝶
刘慧
ZHENG Xiaoxia;XU Jian;TIAN Hongxing;HU Die;LIU Hui(Pharmacy of College,Guiyang College of TCM,Guiyang 550002,China)
出处
《中国药房》
CAS
北大核心
2018年第18期2497-2500,共4页
China Pharmacy
基金
国家苗药工程技术研究中心组建项目(No.2014FU125Q09)
贵州省科学技术基金项目(No.黔科合LH字[2014]7332号)
贵州省普通高等学校工程研究中心项目(No.黔教合KY字[2014]22号)
贵州省优秀青年科技人才培养对象专项资金项目(No.黔科合人字[2015]23号)
贵州省普通高等学校特色重点实验室建设项目(No.黔教合KY字[2016]005)
关键词
妇科再造丸
桨法
体外溶出度
Fuke zaizao pill
Paddle method
in vitro dissolution rate
