中药白矾质量标准改进研究

Improvement of Quality Standard of Alumen

目的 完善中药白矾的质量标准。方法 采用红外光谱法鉴别,替代现行的钾盐、铝盐、硫酸盐三项理化鉴别;采用电感耦合等离子体质谱法同时测定铁、锌、铅、镉、砷、汞、铜的含量,替代现用于检测铁盐、铜盐和锌盐及重金属含量的比色或比浊法;采用离子色谱法进行铵盐检查,替代现行的比色法[2015年版《中国药典(一部)》]或氮测定法[2020年版《中国药典(一部)》];采用电感耦合等离子体质谱法同时测定硫、铝、钾的含量,替代现行测定铝含量的络合滴定法。比较各替代检测方法与现行方法的检测效果。结果 各替代方法经验证,均满足2020年版《中国药典》中方法学验证的要求,且专属性、灵敏度、准确度、检验效率等均优于现行方法。结论 替代方法均为仪器分析,弥补了现行方法的缺陷与不足,大幅提高了质量标准的科学性和有效性,可用于中药白矾的质量控制。

Objective To improve the quality standard of alumen.Methods Instead of the three current physical and chemical identification method,the infrared spectroscopy was used for the identification of potassium salt,aluminum salt and sulfate. Instead of the colorimetry or turbidimetry currently used for detecting the content of iron(Fe),copper(Cu),zinc(Zn) and heavy metals,the inductively coupled plasma mass spectrometry was used for the simultaneous determination of the content of Fe,Zn,lead(Pb),cadmium(Cd),arsenic(As),mercury(Hg) and Cu. Instead of the current colorimetric method [Chinese Pharmacopoeia(2015 Edition,Volume Ⅰ)] or nitrogen determination method [Chinese Pharmacopoeia(2020 Edition,Volume Ⅰ)],the ion chromatography was used to detect ammonium salt. Instead of the complexometric titration method currently used for determining the content of aluminum(Al),the inductively coupled plasma mass spectrometry was used for simultaneous determination of the content of sulfur(S),Al and potassium(K). The detection effect of each alternative detection method with that of the current method was compared.Results After verification,all the alternative methods met the requirements of methodological validation in the Chinese Pharmacopoeia(2020 Edition),and the specificity,sensitivity,accuracy and test efficiency of the methods were better than those of the current methods.Conclusion The alternative methods are all instrumental analysis methods,which make up the shortcomings of the current methods and greatly improve the scientificity and effectiveness of the quality standards,and can be used for the quality control of alumen.