目的:进行了市售雄黄药材及饮片的晶形结构及主成分硫化砷含量的测定,考察了市售雄黄药材及饮片的质量。方法:采用X射线衍射法对市售雄黄药材及饮片进行了物相(晶形)分析,采用《中国药典》(2010年版一部)雄黄项下滴定法测定了雄黄药材及饮片中硫化砷含量。结果:12号、13号雄黄药材主成分是α雄黄(As S)和β雄黄(As4S4)混合体,14号、15号雄黄药材主成分是α雄黄(As S),16号雄黄药材主成分是β雄黄(As4S4),6号雄黄饮片为二氧化硅和α雄黄(As S)的混合体。市售药材中硫化砷含量均在92%~99%范围内,含量均大于90%;雄黄饮片中硫化砷含量均在7%~87%范围内,含量均小于90%。结论:X射线衍射法可以对雄黄进行定性鉴别,市售雄黄饮片整体的质量存在参差不齐的现状。
Objective: The crystal construction and the content of principal component( As S) were determined in order to investigate the quality of realgar in commercially available medicinal materials and decoction pieces. Methods: Crystal construction of realgar was tested by X-ray diffraction,As S content was determined by titration based on the analysis method of realgar recorded in Chinese Pharmacopoeia( 2010edition). Results: The experiments indicated that the twelve and thirteen samples were the mixture of α-realgar( As S) and β-realgar( As4S4); the fourteen and fifteen samples mainly included α-realgar( As S); the sixteen sample contained β-Realgar( As4S4); the six sample was the mixture of silicon dioxide and α-realgar( As S). The contents of realgar ranged from 92% to 99% in the commercially available medicinal materials,and all of them were more than 90%; while the contents of realgar in the decoction pieces were from the range of 7% to 87%,and all of them were less than 90%. Conclusion: X-ray diffraction can be used to identify realgar,and the overall quality of realgar are uneven in commercially available decoction pieces.