今日药学

2020, v.30(09) 616-619

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止痛擦剂中新乌头碱、次乌头碱和乌头碱含量测定研究
Research on the Determination of Mesaconitine,Hypaconitine and Aconitine in Zhitong Liniment

高珊;唐蕾;赵伟国;梁镇标;
GAO Shan;TANG Lei;ZHAO Weiguo;LIANG Zhenbiao;Zhongshan People's Hospital;

摘要(Abstract):

目的建立止痛擦剂中新乌头碱、次乌头碱和乌头碱的含量测定方法。方法采用HPLC法,色谱柱为Eclipse XDB-C_(18)(250 mm×4.6 nm,5μm)。以乙腈-四氢呋喃(25∶15)为流动相A,以0.1 mol·L~(-1)醋酸铵溶液(每1 000 mL加冰醋酸0.5 mL)为流动相B,进行梯度洗脱。检测波长:235 nm;流速:0.8 mL·min~(-1);柱温:30℃。结果高效液相色谱法测定新乌头碱在13.83~276.64μg·mL~(-1)范围内线性关系良好(r=0.999 7),加样回收率为99.47%(n=6,RSD=1.71%);次乌头碱在4.10~82.00μg·mL~(-1)范围内线性良好(r=0.999 6),加样回收率为99.68%(n=6,RSD=3.13%);乌头碱在4.33~86.64μg·mL~(-1)范围内线性关系良好(r=0.999 9),加样回收率为99.27%(n=6,RSD=3.50%)。结论建立的方法简便,准确,重复性好,可有效控制该制剂的质量。
OBJECTIVE To establish the method for the content determination of mesaconitine,hypaconitine and aconitine in Zhitong liniment.METHODS HPLC method was used for the detection.The content were analyzed by Eclipse XDB-C_(18)(250 mm×4.6 nm,5 μm),with the mobile phase A of acetonitrile-tetrahydrofuran(25 ∶15) and the mobile phase B of 0.1 mol·L~(-1) ammonium acetate(containing 0.5 mL glacial acetic acid per 1 000 mL) for gradient elution at a flow of 0.8 mL·min~(-1).The detection wavelength was at 235 nm and column temperature was 30 ℃.RESULTS Mesaconitine linear range was from 13.83 to 276.64 μg·mL~(-1)(r=0.999 7),the average recovery was 99.47%(n=6,RSD=1.71%).The linear range of hypaconitine was 4.10 to 82.00 μg·mL~(-1)(r=0.999 6),the average recovery was 99.68%(n=6,RSD=3.13%).Aconitine has a good linearity at the range of 4.33 to 86.64 μg·mL~(-1)(r=0.999 9),and the average recovery was 99.27%(n=6,RSD=3.50%).CONCLUSION This method is simple,accurate,reproducible and capable of effectively controlling the quality of Zhitong liniment.

关键词(KeyWords): 止痛擦剂;新乌头碱;次乌头碱;乌头碱;高效液相色谱法
Zhitong liniment;mesaconitine;hypaconitine;aconitine;HPLC

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作者(Author): 高珊;唐蕾;赵伟国;梁镇标;
GAO Shan;TANG Lei;ZHAO Weiguo;LIANG Zhenbiao;Zhongshan People's Hospital;

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