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目的通过经典方法对朱砂安神丸(水蜜丸)中朱砂的含量进行测定。方法采用铜试剂滴定的容量法,试样用盐酸与硝酸混合酸(1∶1)分解,在pH>8的氨性溶液中,铜试剂与汞(Ⅱ)生成白色沉淀(二乙胺基二硫代甲酸汞),过量的铜试剂与Cu2+生成黄色沉淀(二乙氨基二硫代甲酸铜),其黄色沉淀可用四氯化碳浓集,以指示终点。结果 3个批次朱砂安神丸中所测得朱砂的平均含量(以硫化汞计算)为14.10%,RSD为0.5%;精密度试验测定,平均含量为14.40%,RSD为0.25%;平均回收率为96.45%,RSD为1.94%。结论本法具有干扰因素少、操作方便的特点。测定范围从万分之几至百分之几十,故适用于本制剂朱砂中硫化汞的含量测定。该方法操作简便、结果准确、重现性好。为将硫化汞含量作为制剂质量控制的指标之一来进一步提升药品质量标准提供了实验依据。
Objective To determine the content of cinnabar in cinnabar Anshen pill (water pill) by classical method. Methods The volumetric method of titration with copper reagent was used. The sample was decomposed by mixed acid (1: 1) with hydrochloric acid and nitric acid, and the white precipitate was formed between copper reagent and mercury (Ⅱ) in ammoniacal solution with pH> 8 Mercury thiomethanesulfonate), an excess of copper reagent forms a yellow precipitate (copper diethylamino dithiocarboxylate) with Cu2 +, and the yellow precipitate can be concentrated with carbon tetrachloride to indicate the end point. Results The average content of cinnabar (calculated as mercuric sulfide) in three batches of cinnabar and Anshen pill was 14.10% and the RSD was 0.5%. The average content was 14.40% and the RSD was 0.25% in the precision test. The average recovery 96.45%, RSD 1.94%. Conclusion This method has the characteristics of less interference and convenient operation. Determination range from very few to tens of percent, it is suitable for the preparation of cinnabar mercury sulfide content determination. The method is simple, accurate and reproducible. In order to mercury sulfide content as one of the indicators of quality control to further improve the quality standards of medicines provided an experimental basis.