去甲斑蝥素片的制备工艺及其含量测定(1)
[摘要] 目的 建立一种去甲斑蝥素片的制备方法，采用HPLC法检测去甲斑蝥素片的含量。 方法 以去甲斑蝥素为主药，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)为黏合剂，以硬脂酸镁为润滑剂，制备去甲斑蝥素片。采用高效液相色谱法(HPLC)检测去甲斑蝥素片的含量；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：20 μl。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蝥素片的制备工艺。 结果 HPLC标准曲线方程：Y=925.374X-1778.8(r=0.9999)；线性范围：20～800 μg/ml。日内精密度RSD：1.880%、0.172%、0.945%；日间精密度RSD：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蝥素片外形美观，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。
[关键词] 去甲斑蝥素片；高效液相色谱；溶出度；均匀设计
[中图分类号] R927 [文献标识码] A [文章编号] 1674-4721(2016)01(c)-0086-04
[Abstract] Objective To establish a preparation method of Norcantharidin tablets，and to detect content of Norcantharidin 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 20 μl.The factors A (starch)，B (MCC) and C (CMS-Na) were selected，U7 (73) uniform design was adopted，and preparation of Norcantharidin tablets was optimized through the dissolution 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%.Coefficient 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., 百拇医药(王钦 薛明道 金智华)
[关键词] 去甲斑蝥素片；高效液相色谱；溶出度；均匀设计
[中图分类号] R927 [文献标识码] A [文章编号] 1674-4721(2016)01(c)-0086-04
[Abstract] Objective To establish a preparation method of Norcantharidin tablets，and to detect content of Norcantharidin 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 20 μl.The factors A (starch)，B (MCC) and C (CMS-Na) were selected，U7 (73) uniform design was adopted，and preparation of Norcantharidin tablets was optimized through the dissolution 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%.Coefficient 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., 百拇医药(王钦 薛明道 金智华)