论文部分内容阅读
目的：建立一种去甲斑螫素片的制备方法,采用HPLC法检测去甲斑螫素片的含量。方法以去甲斑螫素为主药,以淀粉、微晶纤维素（MCC）、乳糖为填充剂,以羧甲基淀粉钠（CMS-Na）为崩解剂,以聚乙烯吡咯烷酮-K30（PVP-K30）为轴合剂,以硬脂酸镁为润滑剂,制备去甲斑螫素片。采用高效液相色谱法（HPLC）检测去甲斑螫素片的含量；HPLC色谱条件为Spherigel ODS-C18色谱柱；流动相：乙腈-pH 3.1磷酸水溶液（10：90）（V／V ）；流速：1.0 ml／min；柱温：25℃；检测波长：210 nm；进样量：20μl。选定A（淀粉）、B（MCC）、C（CMS-Na）为考察因素,采用U7（73）均匀设计,通过溶出度指标优化去甲斑螫素片的制备工艺。结果HPLC标准曲线方程：Y＝925.374X-1778.8（r＝0.9999）；线性范围：20~800μg／ml。日内精密度R SD：1.880％、0.172％、0.945％；日间精密度R SD：1.420％、1.126％、1.468％。低、中、高浓度的回收率分别为（98.77±1.24）％、（100.08±1.14）％、（99.59±0.58）％（n＝5）。均匀设计回归方程为：K＝-0.107-0.004A＋0.017B-0.025C-0.0002B2＋0.007C2（F＝245.312,P﹤0.05）；确定优化处方组成为：淀粉10％、MCC 40％、乳糖43％、CMS-Na 7％；验证得溶出速率常数K为（0.332±0.019）／min。结论按优选处方制备的去甲斑螫素片外形美观,流动性、润滑性、压缩成形性均良好；采用HPLC法可有效控制片剂质量。“,”Objective To establish a preparation method of Norcantharidin tablets,and to detect content of Norcan-tharidin Tablets by using HPLC method. Methods Norcantharidin tablets were prepared with norcantharidin as the main drug,microcrystalline cellulose (MCC) and lactose as the fillers,sodium carboxymethyl starch (CMS-Na) as the disintegrating agent,polyvinylpyrrolidone K30 (PVP-K30) as adhesive.Content of Norcantharidin tablets was detected with the method of HPLC;HPLC chromatographic conditions were: Spherigel ODS C18 chromatographic column;mobile phase:acetonitrile-pH 3.1 phosphoric acid aqueous solution (10:90) (V/V );the flow rate of 1.0 ml/min;column temperature 25℃;detection wavelength of 210 nm;sample quantity 20μl.The factors A (starch),B (MCC) and C (CMS-Na) were se-lected,U7 (73) uniform design was adopted,and preparation of Norcantharidin tablets was optimized through the dissolu-tion index. Results HPLC standard curve equation: Y=925.374X-1778.8 (r=0.9999);linear range: 20~800 μg/ml.The intra-day precision RSD were 1.880%,0.172%,0.945%;inter-day precision RSD were 1.420%,1.126% and 1.468%.Co-efficient of recovery in low,medium and high concentrations were separately (98.77 ±1.24)%, (100.08 ±1.14)%, (99.59 ± 0.58)% (n=5).Uniform design regression equation was K=-0.107-0.004A+0.017B-0.025C-0.0002B2+0.007C2 (F=245.312, P﹤0.05);the optimized prescription composition was 10% starch,40% MCC,43% lactose and 7% CMS-Na;dissolution rate constant K was validated of (0.332 ±0.019)/min. Conclusion Norcantharidin tablets prepared with the optimized prescription preparation are with beautiful shape,good liquidity,lubricity and compression formability;HPLC method can effectively control the quality of tablets.