一种PI3Kδ选择性抑制剂溶出度测定方法的建立  

Establishment of a Dissolution Method of PI3KδSelective Inhibitor

作　　者：屈晓博 王金国 周海峰 夏红梅[1] QU Xiao-bo;WANG Jin-guo;ZHOU Hai-feng;XIA Hong-mei(Anhui University of Chinese Medicine,Hefei 230012,China;Drug Advanced Research Institute of Yangtze Delta,Nantong 226133,China;Haimen Pharma Inc.,Nantong 226133,China)

机构地区：[1]安徽中医药大学,安徽合肥230012 [2]南通市海门长三角药物高等研究院,江苏南通226133 [3]江苏宣泰药业有限公司,江苏南通226133

出　　处：《药物生物技术》2024年第2期141-145,共5页Pharmaceutical Biotechnology

摘　　要：文章建立了具有处方工艺区分力的XT01片溶出测定方法。采用Sunfire C_(18)色谱柱(4.6 mm×50 mm,3.5μm),流动相为0.05%三氟乙酸水溶液(v/v)-0.05%三氟乙酸乙腈溶液(v/v)(75∶25),体积流量1.0 mL/min,检测波长246 nm,柱温30℃,进样量15μL的色谱检测方法。通过考察XT01片在不同溶出介质、表面活性剂、搅拌速度对XT01片溶出行为的影响,筛选具有处方工艺区分力的溶出方法,并对该方法进行专属性、线性、准确度、回收率、溶液稳定性和滤膜吸附的方法学验证。XT01溶出度测定方法为采用桨法,转速75 r/min,37℃,含0.20%十二烷基硫酸钠的pH 6.8磷酸盐溶液为溶出介质,且方法学验证结果均符合测定要求,XT01在4.4~26.8μg/mL范围内线性关系良好。本溶出方法可有效应用于XT01片的溶出度检测,能够区分不同处方工艺之间溶出行为差异。The main purpose of this study is to establish a dissolution method for XT01 tablets that can distinguish from different for-mulations and process parameters.The HPLC method adopted a Sunfire C_(18)column(4.6 mm×50 mm,3.5μm)and a mobile phase containing of a 0.05%aqueous solution of trifluoroacetic acid(v/v)and a 0.05%solution of trifluoroacetic acid in acetoni-trile(v/v)(75∶25)at flow rate of 1.0 mL/min.The detection wavelength was set at 246 nm,the column temperature was main-tained at 30℃,and the injection volume was 15μL.The discriminative dissolution method was developed by evaluation of the effects of different dissolution media,surfactants,and stirring speed on the dissolution behavior of XT01 tablets,and the method was validated in items of specificity,linearity,accuracy,recovery,solution stability,and filter bias.The paddle method was used to deter-mine XT01 dissolution at 75 r/min and 37°C,with a pH 6.8 phosphate solution containing 0.20%sodium dodecyl sulfate as the dissolution medium.The method validation results met the requirements,and XT01 exhibited good linearity in the range of 4.4 to 26.8μg/mL.The dissolution method is suitable for testing the dissolution of XT01 tablets and can discriminate the dissolution behaviors of tablets produced using different formulations and process parameters.

关 键 词：XT01片 溶出度 区分力 方法开发 方法验证 高效液相色谱 

分 类 号：R927.1[医药卫生—药学]