盐酸小檗胺片溶出度测定方法的建立及其体外溶出性能评价  

Establishment of Dissolution Tests and Evaluation of Dissolution Performance for Berbamine Hydrochloride Tablets

作　　者：董宁 刘慧颖 孙立新[1] DONG Ning;LIU Huiying;SUN Lixin(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Liaoning Institute for Drug Control,Shenyang 110036,China)

机构地区：[1]沈阳药科大学药学院,沈阳110016 [2]辽宁省药品检验检测院,沈阳110036

出　　处：《中国药房》2018年第17期2356-2359,共4页China Pharmacy

基　　金：国家药典委员会药品标准提高课题(No.239)

摘　　要：目的:建立盐酸小檗胺片溶出度的测定方法,评价5家企业样品的批内质量。方法:采用高效液相色谱法测定盐酸小檗胺浓度并计算累积溶出度。色谱柱为Agilent C18,流动相为0.02 mol/L磷酸氢二钾溶液(含0.2%三乙胺,磷酸调p H至6.8)-乙腈(60∶40,V/V),流速为1.0 m L/min,检测波长为282 nm,柱温为35℃,进样量为40μL。采用桨法,以累积溶出度为指标,筛选溶出介质(水、p H 5.5醋酸-醋酸钠缓冲液、p H 6.8磷酸盐缓冲液)和转速(50、75 r/min),确定溶出度测定的条件。绘制5家企业样品的溶出曲线,比较批内均一性。结果:盐酸小檗胺检测质量浓度线性范围为3.96~257.40μg/m L(r=0.999 9),精密度、稳定性(8 h)、重复性、耐用性试验的RSD均<2.0%(n=5或n=6),平均回收率为98.6%(RSD=1.64%,n=9)。在3种溶出介质及2种转速下药物累积溶出度无明显差异,最终确定水为溶出介质、转速为50 r/min。在5家企业样品中,只有1家企业的样品批内均一性较好。结论:所建立的溶出度测定方法简便易行、准确度高,可用于盐酸小檗胺片中盐酸小檗胺的溶出度测定;部分企业需进一步提高药品质量。OBJECTIVE:To establish a method for determining the dissolution of Berbamine hydrochloride tablets,and to evaluate the intra-batch quality of samples from 5 enterprises.METHODS:The concentration of berbamine hydrochloride was determined by HPLC and accumulative dissolution was calculated.The determination was performed on Agilent C18 column with mobile phase consisted of 0.02 mol/L dipotassium hydrogen phosphate solution(containing 0.2%triethylamine,pH adjusted to 6.8 with phosphoric acid)-acetonitrile(60∶40,V/V)at the flow rate of 1.0 mL/min.The detection wavelength was set at 282 nm.The column temperature was set at 35℃,and sample size was 40μL.With paddle method,using accumulative dissolution as index,the medium(water,pH 5.5 acetic acid-sodium acetate buffer solution,pH 6.8 phosphate buffer solution)and rotation speed(50,75 r/min)were selected to establish the determination condition of dissolution.The dissolution curves of 5 enterprises were drawn to compare the intra-batch uniformity of samples.RESULTS:The linear range of berbamine hydrochloride were 3.96-257.40μg/mL(r=0.999 9).RSDs of precision,stability(8 h),reproducibility and durability tests were all lower than 2.0%(n=5 or n=6).The average recoveries were 98.6%(RSD=1.64%,n=9).The accumulative dissolution of samples in 3 kinds of mediums at 2 kinds of rotation speeds had no obvious differences.The optimal determination condition was water as medium at rotation speed of 50 r/min.Of all the five enterprises,intra-batch uniformity of sample was satisfied in only on enterprise.CONCLUSIONS:Established method is simple,feasible and accurate,and it can be used to determine the dissolution of berbamine hydrochloride in Berbamine hydrochloride tablets.Some enterprises should make further efforts to improve the quality of medicines.

关 键 词：盐酸小檗胺片 桨法 溶出度 高效液相色谱法 

分 类 号：R927.1[医药卫生—药学]