氟哌啶醇片溶出度测定方法的改进  

Improvement of Determination Method of the Dissolution of Haloperidol Tablets

作　　者：余倩[1] 段永生[1] 杜凯[1] 刘珊珊[1] 车宝泉[1] 

机构地区：[1]北京市药品检验所,北京100035

出　　处：《中国药房》2014年第1期73-75,共3页China Pharmacy

摘　　要：目的：建立氟哌啶醇片新的溶出度测定方法。方法：溶出度法由《中国药典》的小杯法改为篮法，以盐酸溶液900ml代替200ml为溶出介质，转速为100r／min；检测方法由原来的紫外分光光度法改为高效液相色谱法，色谱柱为IntersilC18，流动相为甲醇．0．05mol／L磷酸二氢钾溶液（60：40，pH4．0），流速为1．0ml／min，检测波长为248nm，柱温为30℃，进样量为50p1。同时比较两种方法测定6批样品的溶出度结果。结果：氟哌啶醇检测质量浓度线性范围为0．531～4．248μg／ml（r=O．9999），平均回收率为99．58％（RsD=0．46％。n=3）；样品的溶出时间由原来的45min缩短至30min，限度由原来的70％提高到80％。新方法与原方法相比溶出量更高，RSD更小，样品溶出均一性更好。结论：新方法提高了溶出度检测的专属性和准确性，较好地体现了片剂间的差异。OBJECTIVE： To establish the method for the determination of dissolution of Haloperidol tablets. METHODS： The dissolution experiment adopted rotating basket method in Chinese Pharmacopeia instead of small vessel method, using hydrochloric acid solution 900 ml instead of 200 ml as solvent and rotating speed of 100 r/min. The determination method changed from UV to HPLC. The analytical column was Intersil C18 column with mobile phase consisted of methanol-0.05 mol/L potassium dihydrogen phosphate solution （60：40, pH adjusted to 4.0） at the flow rate of 1.0 ml/min. The detection wavelength was set at 248 nm, and column temperature was 30 ℃. The injection volume was 50 μl. The detection methods for the dissolution of 6 batches of samples were compared. RESULTS： The linear range of haloperidol were 0.531-4.248 μg/ml （r=0.999 9） with an average recovery of 99.58% （RSD=0.46%, n=3）. The dissolution time for the sample decreased to 30 min from the previous 45 min, and the limita- tion rate increased from 70% to 80%. Compared with previous method, new method showed higher dissolution, lower RSD and better homogeneity. CONCLUSIONS： The method improves the accuracy and specificity for dissolution detection. The improved dissolution method is more discriminating among different tablets than before.

关 键 词：氟哌啶醇片 溶出度测定 方法改进 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]