[关键词]
[摘要]
目的 建立藏药佐塔中单质硫和HgS含量测定方法,并根据质量守恒定律制定合理限度,为其质量控制提供依据。方法 采用结晶法分离纯化佐塔中单质硫,X射线单晶衍射进行结构鉴定;高效液相色谱法测定佐塔样品中单质硫含量,硫氰酸铵容量法测定HgS含量;根据佐塔炮制过程中水银和硫黄等比例加入特点,采用质量守恒定律计算单质硫和HgS限度及八金八矿灰添加量。结果 佐塔中分离得到的单质硫属斜方晶系S8,空间群Fddd,晶胞参数a=1.046 2(9) nm,b=1.286 3(9) nm,c=2.448 3(2) nm,V=3.294 8(5) nm3,α=β=γ=90°,Z=16,F(000)=2049;9批佐塔中单质硫质量分数在35.35%~40.66%,HgS质量分数在53.54%~56.33%;根据Hg+S→HgS化学反应方程式及质量守恒定律可推算,佐塔中单质硫和HgS最大限量分别为42.0%和58.0%,9批佐塔中八金八矿灰添加量为2.96%~8.33%。结论 通过测定佐塔中单质硫和HgS含量,不仅可较全面评价佐塔质量,还能计算八金八矿灰等辅料加入量,为其质量标准建立及后续炮制工艺规范化研究提供参考。
[Key word]
[Abstract]
Objective The study aims to establish a method for the determination of contents of elemental sulfur (S) and HgS in Zuota, a Tibetan medicine, and set a reasonable limitation of their contents based on the law of conservation of mass, so as to provide a basis for its quality control. Methods The method of crystallization method was used to separate and purify the sulfur in Zuota, and the method of X-ray diffraction was used for its structure identification. The method of HPLC and NH4SCN titration method were used to determine the contents of S and HgS in Zuota, respectively. According to the characteristics of mercury and sulfur added at the same proportion in the process of Zuota, the limitation of S and HgS, and the added content of eight kinds of metal ash and eight mineral ash were calculated by the law of conservation of mass. Results S isolated from Zuota belonged to orthorhombic system of S8, the spatial group of Fddd. The cell parameters were a=1.046 2(9) nm, b=1.286 3(9) nm, c=2.448 3(2) nm, V=3.294 8(5) nm3, α=β=γ=90°, Z=16, F(000)=2049. The contents of S and HgS in nine batches of Zuota were 35.35%-40.66% and 53.54%-56.33%, respectively. According to the chemical reaction equation of Hg + S→HgS and the law of conservation of mass, the max limited contents of S and HgS in Zuota should not more than 42.0% and 58.0%, respectively. The additive amount of eight kinds of metal ash and eight mineral ash in nine batches of Zuota was 2.96%-8.33%. Conclusion By determining the contents of S and HgS in Zuota, not only the quality of Zuota could be assessed comprehensively, but also the amount of eight kinds of metal ash, eight mineral ash and other things which were used as auxiliary materials could be speculated. This study can provide a useful reference for the research on the standardization of processing technology and establishment of quality standards of Zuota.
[中图分类号]
R283.6
[基金项目]
国家重点研发计划项目(2018YFC1708005);四川省药品监督管理局项目(510201201810173);西南民族大学中央高校基本科研业务费专项资助(2020NGD01)