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目的:建立追风舒筋活血片中马钱子碱、士的宁的含量测定方法。方法:应用高效液相色谱法测定,色谱柱为Agilent-SB C_(18)柱(250 mm×4.6 mm,5μm),以乙腈-0.01 mol·L~(-1)庚烷磺酸钠与0.02 mol·L~(-1)磷酸二氢钾等量混合溶液(用10%磷酸调节p H至2.8)(21∶79)为流动相,检测波长为260 nm,流速为1.0 ml·min~(-1),柱温为35℃,进样量为10μl。结果:马钱子碱和士的宁的线性范围分别为0.011 0~0.219 6 mg·ml~(-1)(r=0.999 4)、0.010 1~0.202 8 mg·ml~(-1)(r=0.999 7);平均加样回收率分别为98.24%(RSD=1.54%)、97.92%(RSD=1.49%)(n=6)。结论:该方法简便易行、准确、重复性好,可用于追风舒筋活血片的质量控制。
Objective: To establish a method for determining the content of brucine and strychnine in Herring Shujinhuoxue tablets. Methods: The HPLC-MS method was used for the determination of trace compounds in the chromatographic column with Agilent-SB C 18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile-0.01 mol·L -1 heptane sulfonate and 0.02 mol·L -1 potassium dihydrogen phosphate (pH was adjusted to 2.8 with 10% phosphoric acid) (21:79) as the mobile phase at a detection wavelength of 260 nm at a flow rate of 1.0 ml · min -1 -1), the column temperature was 35 ℃, the injection volume was 10μl. Results: The linear ranges of brucine and strychnine were 0.011 0-0.219 6 mg · ml -1 (r = 0.999 4), 0.010 1 ~ 0.202 8 mg · ml -1 (r = 0.999 7). The average recoveries were 98.24% (RSD = 1.54%) and 97.92% (RSD = 1.49%) (n = 6), respectively. Conclusion: The method is simple, accurate, reproducible and can be used for the quality control of Qifeng Shujinhuoxue Tablet.