目的建立冠心苏合丸（Guanxin Suhe Pill，GXSHP）HPLC内标定量指纹图谱，用内标定量指纹图谱法选出冠心苏合丸对照制剂，为冠心苏合丸的质量控制提供对照制剂控制法。方法采用AgilentPoroshell 120SBC18色谱柱（150mm×4．6mm，2．...目的建立冠心苏合丸（Guanxin Suhe Pill，GXSHP）HPLC内标定量指纹图谱，用内标定量指纹图谱法选出冠心苏合丸对照制剂，为冠心苏合丸的质量控制提供对照制剂控制法。方法采用AgilentPoroshell 120SBC18色谱柱（150mm×4．6mm，2．7μm），流动相为水-甲醇（均含0．2％醋酸），梯度洗脱，体积流量0．5mL／min，柱温（25．00±0．15）℃，紫外检测波长为275nm，进样量5此。采用内标定量指纹法整体鉴定12批次GXSHP（S1～S12）质量，根据本方法评价结果选出冠心苏合丸对照制剂。结果以内标物峰为参照峰，确定36个共有指纹峰，以加入固定浓度内标为基准建立了GXSHP-HPLC内标定量指纹图谱。用内标定量指纹法鉴别出s3、s5～s7、s9质量极好，s4、S8、s10、s11质量很好，s1、s2质量好，S12质量为劣，根据该方法评价结果，最终确定s3、s5～S7、S9可作为冠心苏合丸对照制剂。结论内标定量指纹法可以减少对照品的使用，校正指纹图谱变化，提高测定结果的准确性，选出的对照制剂生成冠心苏合丸对照制剂指纹图谱可用于大批量冠心苏合丸的质量控制，具有重大的实际应用意义。展开更多
The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quan...The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.展开更多
文摘目的建立冠心苏合丸（Guanxin Suhe Pill，GXSHP）HPLC内标定量指纹图谱，用内标定量指纹图谱法选出冠心苏合丸对照制剂，为冠心苏合丸的质量控制提供对照制剂控制法。方法采用AgilentPoroshell 120SBC18色谱柱（150mm×4．6mm，2．7μm），流动相为水-甲醇（均含0．2％醋酸），梯度洗脱，体积流量0．5mL／min，柱温（25．00±0．15）℃，紫外检测波长为275nm，进样量5此。采用内标定量指纹法整体鉴定12批次GXSHP（S1～S12）质量，根据本方法评价结果选出冠心苏合丸对照制剂。结果以内标物峰为参照峰，确定36个共有指纹峰，以加入固定浓度内标为基准建立了GXSHP-HPLC内标定量指纹图谱。用内标定量指纹法鉴别出s3、s5～s7、s9质量极好，s4、S8、s10、s11质量很好，s1、s2质量好，S12质量为劣，根据该方法评价结果，最终确定s3、s5～S7、S9可作为冠心苏合丸对照制剂。结论内标定量指纹法可以减少对照品的使用，校正指纹图谱变化，提高测定结果的准确性，选出的对照制剂生成冠心苏合丸对照制剂指纹图谱可用于大批量冠心苏合丸的质量控制，具有重大的实际应用意义。
文摘The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.
