消癥止痛凝胶贴膏指纹图谱及体外释放度研究

Study on fingerprint and in vitro release of Xiaozheng-Zhitong cataplasm

目的建立评价消癥止痛凝胶贴膏制备工艺重现性的方法。方法采用指纹图谱技术及体外释放度试验对消癥止痛凝胶贴膏制备工艺的重现性进行评价。采用HPLC法建立消癥止痛凝胶贴膏的指纹图谱,色谱柱为Agilent HC-C18色谱柱(4.6 mm×250 mm,5μm);检测波长280 nm;流速1 ml/min;柱温25℃;流动相为乙腈-0.2%磷酸水溶液,梯度洗脱。建立HPLC法测定延胡索乙素含量的方法,并采用垂直式Franz扩散池法考察其体外释放度。结果10批消癥止痛凝胶贴膏与对照图谱的相似度均在0.95以上;消癥止痛凝胶贴膏中延胡索乙素24 h累积释放量为0.23 mg,8 h累积释放率为91.54%,且6份样品各时间点的RSD值均<3%。结论应用指纹图谱技术及体外释放度建立了消癥止痛凝胶贴膏制备工艺重现性的评价方法,可为贴膏剂制备工艺重现性的评价提供参考和依据。

Objective To establish a method of evaluating the reproducibility of the preparation process of Xiaozheng-Zhitong cataplasm.Methods Used fingerprint spectrum technology and in vitro release test to evaluate the reproducibility preparation process of Xiaozheng-Zhitong cataplasm.By using HPLC to establish the fingerprint of Xiaozheng-Zhitong cataplasm.The chromatographic column was an Agilent HC-C18 column(4.6 mm×250 mm,5μm);the detection wavelength was 280 nm;the flow rate was 1 ml/min;the column temperature was 25℃.The mobile phase was acetonitrile-0.2%phosphoric acid aqueous solution,used gradient elution method.An HPLC method for the determination of tetrahydropalmatine content was established,and the vertical Franz diffusion cell method was used to investigate its in vitro release.Results The results showed that the similarity between the 10 batches of Xiaozheng-Zhitong cataplasm and the control map was above 0.95,indicating that the process of Xiaozheng-Zhitong cataplasm was stable and feasible;the cumulative release amount of tetrahydropalmatine was 0.23 mg in 24 hours,and the cumulative release rate in 8 hours was 91.54%,and the RSD of 6 samples at each time point was<3%.Conclusion The method of evaluating the reproducibility of the preparation process of Xiaozheng-Zhitong cataplasm was established by using fingerprint technology and in vitro release;it can provide a reference and scientific basis for the evaluation of the reproducibility of the preparation process of the plaster.