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粉末X射线衍射法测定消咳宁片中碳酸钙含量
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作者 张建平 孙倩男 +1 位作者 周雪梅 王栋 《分析测试技术与仪器》 CAS 2022年第4期463-468,共6页
采用粉末X射线衍射法(PXRD)快速测定中成药消咳宁片中碳酸钙含量.采用全谱拟合内标定量法,以ZnO为内标物,使用Cu Kα射线,电压为40 kV,电流为45 mA,扫描类型为Coupled Two Theta/Theta,扫描模式为Continuous PSD fast,衍射角(2θ)扫描范... 采用粉末X射线衍射法(PXRD)快速测定中成药消咳宁片中碳酸钙含量.采用全谱拟合内标定量法,以ZnO为内标物,使用Cu Kα射线,电压为40 kV,电流为45 mA,扫描类型为Coupled Two Theta/Theta,扫描模式为Continuous PSD fast,衍射角(2θ)扫描范围8°~40°,步长0.02°.扫描获得PXRD图谱,通过全谱分析(TOPAS)软件进行内标定量分析得到碳酸钙的质量分数.方法学验证结果,方法的平均加标回收率为98.9%[相对标准偏差(RSD)为1.0%,n=6],模拟样采用低中高三水平进行验证,测得回收率平均值为96.9%(RSD=1.0%,n=6).重复性测定RSD为1.2%(n=6). X射线衍射法快速、灵敏、专属性强,全谱拟合内标定量法的准确度、重复性良好,可以解决消咳宁片中碳酸钙含量测定的难题. 展开更多
关键词 粉末X射线衍射 全谱拟合内标定量法 消咳宁片 碳酸钙
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Determination the content of gypsum fibrosum in Xiaokening tablets by powder X ray diffraction method 被引量:2
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作者 Jianping Zhang Xinxin Feng Dong Wang 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2019年第3期186-194,共9页
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
关键词 Powder X ray diffraction Full spectrum fitting internal standard quantitative method Xiaokening tablet Gypsum fibrosum
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