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目的:建立中药紫石英专属性强的含量测定方法。方法:利用药典法、扣减法、酸溶法及X-粉末衍射法对38批紫石英样品进行含量测定,并利用X-粉末衍射法对样品进行物相分析。结果:物相分析结果显示,23批样品为紫石英正品,其X-粉末衍射图谱峰形尖锐简单,除氟化钙外含有少量的石英、铁等杂质;13批样品为紫石英不合格品,其X-粉末衍射图谱峰形尖锐复杂,除氟化钙外含有大量的方解石、石膏及云母族等矿物杂质;2批样品为紫石英伪品,其X-粉末衍射图谱峰形尖锐复杂,主要含有大量的碳酸盐类矿物杂质。含量测定结果显示,正品紫石英样品中氟化钙含量,X-粉末衍射法分析结果略高于药典法结果,有的可达100%,紫石英不合格品与伪品X-粉末衍射法分析结果远远小于药典法结果,表明X-粉末衍射法为半定量分析,此方法具有一定的不确定性;药典法测定结果实际为样品中包含碳酸钙等杂质在内的总钙含量,测定结果均有误差(RSD>2%);酸溶法存在二次滴定,且操作繁琐;扣减法数据在氟化钙含量较高杂质含量较低时,其数据接近药典法,当氟化钙含量较低,杂质含量较高时,其数据接近酸溶法,扣减法测定数据在药典法和酸溶法之间。结论:扣减法准确度高,专属性强。建议《中华人民共和国药典》将扣减法作为中药紫石英的含量测定方法。
Objective: To establish a method for the determination of the high specificity of Chinese medicine Amethyst. Methods: Thirty-eight batches of amethyst samples were determined by pharmacopoeial method, subtractive method, acid-solubilizing method and X-ray powder diffractometry. The phase of the samples was analyzed by X-ray powder diffraction. Results: The results of phase analysis showed that the 23 batches of samples were genuine purple quartz samples. The X-ray powder diffraction patterns of the samples were sharp and simple. A small amount of quartz, iron and other impurities were contained except calcium fluoride. , X-ray powder diffraction pattern sharp sharp complex, except calcium fluoride contains a large number of calcite, gypsum and mica and other mineral impurities; two batches of samples for the purple quartz counterfeit goods, its X-ray powder diffraction pattern sharp sharp complex, Contains a large number of carbonate mineral impurities. The content of calcium fluoride and X-ray powder diffraction analysis showed that the content of calcium fluoride and X-ray powder diffraction analysis of genuine purple quartz were slightly higher than those of the pharmacopoeia, some of them were up to 100%. The results of X-ray powder diffraction The results are far less than the results of the Pharmacopoeia, indicating that the X-powder diffraction method for semi-quantitative analysis, this method has some uncertainty; the results of the Pharmacopoeia determination of the actual sample containing calcium carbonate and other impurities, including the total calcium content, the determination results (RSD> 2%). There was a second titration in acid-soluble method and the operation was cumbersome. The data of deduction method was close to that of the pharmacopoeia when the content of calcium fluoride was relatively high and the content of calcium fluoride Lower, high impurity content, the data close to the acid-soluble method, subtraction method measured data between the Pharmacopoeia and acid-soluble method. Conclusion: deduction method with high accuracy and specificity. Proposed “People’s Republic of China Pharmacopoeia” deduction method as the determination of the content of Chinese medicine purple quartz.