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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: To determine the crystal structure and the content of arsenic sulfide in commercially available realgar and its medicinal herbs, the quality of commercially available realgar and its medicinal herbs were studied. Methods: X-ray diffraction (XRD) was used to analyze the phase (crystal form) of commercially available realgar herbs and Pieces. The content of arsenic sulfide in Radix realgar and Pieces was determined by realgar titration under “Chinese Pharmacopoeia” (2010 edition). Results: The main constituents of No12 and No.13 realgar were As mixed with As4S4. The main constituents of No.14 and No.15 realgar were As-S, main components of No.16 realgar Is beta realgar (As4S4), and realgar realgar 6 is a mixture of silica and alpha realgar (AsS). The content of arsenic sulfide in the commercially available medicinal materials is in the range of 92% -99%, and the content is more than 90%. The content of arsenic sulfide in the realgar slices is in the range of 7% -87%, all less than 90%. Conclusion: X-ray diffractometry can be used for the qualitative identification of realgar, and the quality of marketed realgar has the uneven quality.