朱砂锆球水飞工艺及质量评价研究

Research on zirconium ball water grind processing of Cinnabaris and quality evaluation

目的建立适用于工业生产的朱砂锆球水飞工艺,提升朱砂质量。方法以外观性状、粉体特征、工艺收率及硫化汞含量为指标,采用线性插值法将各指标数据进行标准化转换,根据层次分析法确定各指标权重系数综合评分,通过单因素结合星点设计-响应面法的方法对锆球水飞朱砂工艺进行考察;借助扫描电镜(SEM)、激光粒度检测、热重分析(TG)、拉曼光谱及电感耦合等离子体质谱(ICP-MS)对比朱砂炮制前后质量差异,初步探讨朱砂锆球水飞炮制机制。结果确定了朱砂锆球水飞的最佳炮制工艺:取净朱砂,置研磨筒中,加入直径1、2、3、4 mm研磨球400 g,加水450 mL,研磨120 min,再加水800 mL,搅拌,倾出混悬液,残渣按上述方法再次操作,合并混悬液,静置72 h,分取沉淀,40℃干燥,研散。并采用16批朱砂药材对优选的锆球水飞工艺进行验证。探索了现代技术从微观性状、化学成分组成、结构等多方面对于矿物药质量的综合评价方法。结论朱砂锆球水飞工艺简化了传统水飞次数,保留了传统水飞的特点,量化了关键操作技术点的参数,经验证工艺条件稳定、合理、可行。朱砂锆球水飞技术起到了良好的除杂、提纯、减毒的作用。

Objective To establish a Cinnabaris zirconium ball water grind processing suitable for industrial production to improve the quality of Cinnabaris decoction pieces.Methods Taking appearance properties,powder characteristics,process yield and mercury sulfide content as indicators,according to the analytic hierarchy process,the comprehensive score of the weight coefficient of each index was determined,and the zirconium ball water flying Cinnabaris process was investigated through the single factor combined with the star point design-response surface method;With the help of scanning electron microscope(SEM),particle size detection,thermogravimetric analysis(TG),Raman spectroscopy and inductively coupled plasma mass spectrometry(ICP-MS)to compare the quality difference of Cinnabaris before and after the processing,and preliminarily discussed the mechanism of Cinnabaris zirconium ball water grind processing.Results The optimal concoction processing for zirconium ball water grind of Cinnabar was determined by taking a certain amount of Cinnabaris,accurately weighing it,and placing it in the grinding cylinder,adding 400 g of grinding balls with diameters of 1,2,3,4 mm,adding 450 mL of water,grinding for 120 min,then adding 800 mL of water,stirring,and pouring out the suspension,and the preferred zirconium ball water grind processing was validated using 16batches of Cinnabaris herbs.A comprehensive evaluation method of modern technology for the quality of mineral medicine with various aspects such as microscopic properties,chemical composition and structure was explored.Conclusion The Cinnabaris zirconium ball water grind process simplifies the traditional water grind times,retains the characteristics of the traditional water grind,quantifies the parameters of the key operating technology points,and the process conditions which have been validated are stable,reasonable and feasible.Cinnabaris zirconium ball water grind technology has played a good role in impurity removal,purification and attenuation.