响应面法优化《中国药典》大青叶含量测定方法及差异分析  

Optimization of determination method and difference analysis of Isatidis folium in Chinese Pharmacopoeia by response surface method

作　　者：王晓蕾 孙慧珠 刘晓明 苏建 刘永利 WANG Xiaolei;SUN Huizhu;LIU Xiaoming;SU Jian;LIU Yongli(Department of Traditional Chinese Medicine,Hebei Institute for Drug and Medical Device Control,Hebei Shijiazhuang 050227,China;Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicinal Materials,State Food and Drug Administration,Hebei Shijiazhuang 050227,China;Drug Evaluation Department Two,Hebei Drug Evaluation Center,Hebei Shijiazhuang 050000,China)

机构地区：[1]河北省药品医疗器械检验研究院中药室,河北石家庄050227 [2]国家药监局中药材质量监测评价重点实验室,河北石家庄050227 [3]河北省药品评审中心药品审评二部,河北石家庄050000

出　　处：《中国医院药学杂志》2024年第5期557-563,共7页Chinese Journal of Hospital Pharmacy

基　　金：国家药品标准提高研究课题(编号:2017Z398);河北省省级科技计划(编号:21372502D)。

摘　　要：目的:优化《中国药典》大青叶质量标准含量测定的指标及方法。方法:优选提取溶剂,再以N,N-二甲基甲酰胺(DMF)溶液的磷酸体积分数、提取方式与液料比为考察因素,以靛蓝、靛玉红含量为响应值,采用Box-Behnken响应面法分析因素间交互作用。通过方法学验证、预测值验证、方法对比验证方法优势。结果:以含磷酸的DMF溶液为提取溶剂,明确各因素对响应值的影响为磷酸体积分数>振摇时间>液料比,最终确定供试品溶液制备的最优条件,0.5 g大青叶加5%磷酸的DMF溶液25 mL,振摇提取40 min。采用高效液相色谱法同时测定靛蓝与靛玉红含量,线性关系、重复性、回收率、耐用性良好。结论:将5%磷酸的DMF溶液作为大青叶的提取溶剂,有效提升了靛蓝、靛玉红的提取效率及稳定性,解决了现行标准含量测定项指标单一、方法繁琐的问题,可用于控制大青叶药材及饮片的质量。OBJECTIVE To optimize the quality standard and content determination method for Isatidis folium in Chinese Pharmacopoeia.METHODS Extraction solvent was optimized.Taking the volume fraction of phosphoric acid in N,Ndimethylformamide(DMF)solution,the extraction method and the liquid material ratio as the investigation factors,and the contents of indigo and indirubin as the response values,the Box-Behnken response surface method was applied to analyzing the interaction among the factors.The method verification,prediction value verification and method comparison were used to verify the method advantages.RESULTS DMF solution containing phosphoric acid was used as the extraction solvent.The influence order of each factor from high to low on the response value was the volume fraction of phosphoric acid,the shaking time and the liquid material ratio.Finally,the optimal conditions for the preparation of the test solution were determined as follows:0.5 g of Isatidis folium,adding 25 ml of DMF solution with 5%phosphoric acid,shaking for 40min.A method for the simultaneous determination of indigo and indirubin by high performance liquid chromatography(HPLC)was developed.Linear relationship,repeatability,recovery and durability were all good.CONCLUSION 5%Phosphoric acid in DMF was used as the extraction solvent for Isatidis folium for the first time.It can effectively improve the extraction efficiency and stability of indigo and indirubin,solve the problems of single index and complicated method of the current standard content determination item,and can be used to control the quality of Isatidis folium.

关 键 词：大青叶 靛蓝 靛玉红 高效液相色谱法 Box-Behnken响应面法 

分 类 号：R917[医药卫生—药物分析学]