双乌止痛酊质量标准研究

摘要

目的 制订双乌止痛酊的质量标准.方法 采用薄层色谱法对双乌止痛酊中的制天南星、当归及苯甲酰次乌头原碱进行定性鉴别,同时对制剂中的毒性成分乌头碱进行限量检查;采用高效液相色谱法测定苯甲酰新乌头原碱含量,色谱柱选用Inertsustain C18柱(250 mm×4.6 mm,5μm),以乙腈-0.02 mol/L的磷酸二氢钠(25:75)为流动相,检测波长为230 nm,柱温为30℃,流速为1.0 mL/min.结果 双乌止痛酊中制天南星、当归及苯甲酰次乌头原碱的定性鉴别专属性强,乌头碱限量测定符合规定;苯甲酰新乌头原碱的检测质量浓度在0.01244～0.09952 g/L(r=1.0000,n=5)范围内与峰面积线性关系良好,平均加样回收率为99.36％,RSD=2.45％(n=9).结论 该方法操作简单,准确可靠,可用于双乌止痛酊的质量控制.%Objective To establish the quality standard of Shuangwu Zhitong Tincture. Methods TLC method was adopted for the quali-tative identification of Rhizoma Arisaematis,Angelica Sinensis and benzoylhypaconine in Shuangwu Zhitong Tincture and the limited quantity of aconitine was determined. HPLC method was used to determine the content of benzoylmesaconitine in Shuangwu Zhitong Tincture,the Inertsustain C18 column (250 mm × 4. 6 mm,5 μm)was adopted,the mobile phase system was acetonitrile-0. 02 mol/L NaH2PO4 (25 :75),the detection wavelength was set at 230 nm, the column temperature was 30 ℃, and the flow rate was 1. 0 mL/min. Results The qualitative identification of Rhizoma Arisaematis,Angelica Sinensis,and benzoylhypaconine in Shuangwu Zhitong Tincture was specific,the limited quantity of aconitine accorded with the regulations. The liner range of benzoylmesaconitine was 0. 01244-0. 09952 g/L,r=1. 0000 ( n=5),and the average recovery was 99. 36％,RSD=2. 45％(n=9). Conclusion The method is simple, accurate and reliable,which can be used for the quality control of Shuangwu Zhitong Tincture.