牛黄清心丸(局方)中朱砂和雄黄的含量测定

Determination of Cinnabar and Realgar in Niuhuang Qingxin Pills(Pharmacopoeia)

目的建立牛黄清心丸(局方)中朱砂和雄黄的含量测定方法。方法先对牛黄清心丸进行硝化处理,运用氧化还原滴定法分别以硫氰酸铵滴定液和碘滴定液对制剂中朱砂和雄黄的主要成分硫化汞和二硫化二砷进行定量分析。结果硫化汞取样量在19.8～99 mg范围内与硫氰酸铵滴定液消耗体积呈良好的线性关系,回归方程为Y=85.5 X+0.046,r=0.999,平均加样回收率为101.07%,RSD为2.21%,硫化汞含量为57.75 mg/丸;二硫化二砷取样量在9.5～47.5 mg范围内与碘滴定液消耗体积呈良好的线性关系,回归方程为Y=171.83 X-0.050 9,r=0.999,平均加样回收率为101.08%,RSD为1.10%,二硫化二砷含量为22.91 mg/丸。结论所建立的方法可靠、准确性高、专属性强,可进一步控制该制剂的毒性成分含量。

Objective To establish a determination method of cinnabar and realgar in Niuhuang Qingxin Pills （Pharmacopoeia）. Methods Niuhuang Qingxin Pills was firstly nitrified. The main components mercuric sulfide and arsenic disulfide in cinnabar and realgar in the preparation were performed the quantitative analysis by tbe oxidation- reduction titration with ammonium thiocyanate and iodine titration solutions respectivey. Results Mercury sulfide showed good linear relation in the range of 19.8-99 mg with the consumption volume of ammonium thiocyanate titrant,the regression equation Y=85.5X＋0. 046（r=0. 999）,the average recovery rate was 101.07% with RSD of 2.21% ,the mercuric sulfide content was 57.75 mg per pill. Arsenic disulfide showed in good linear relation in the range of 9.5- 47.5 mg with the consumption volume of iodine titrant,the regression equation Y = 171.83 X- 0. 050 9（ r = 0. 999）,the average recovery rate was 101.08% , RSD 1.10% , the arsenic disulfide content was 22.91 mg per pill. Conclusion The established method is reliable,highly accurate,strongly specific and can further control the contents of the toxic ingredients in the preparation.