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目的:建立同时测定苯甲酸利扎曲普坦含量和有关物质的RP-HPLC离子对梯度洗脱法。方法:色谱柱:Phenomenex C18(250 mm×4.6 mm,5μm);流动相:A相为乙腈-5 mmol.L-1庚烷磺酸钠溶液(24:76,醋酸调pH3.4),B相为乙腈-5mmol.L-1庚烷磺酸钠溶液(38:62,醋酸调pH3.4),梯度洗脱;流速:1.0 mL.min-1;柱温:30℃;检测波长:227 nm。结果:利扎曲普坦峰与相邻杂质峰的分离符合要求;苯甲酸利扎曲普坦在0.02～16μg.mL-1浓度范围内线性关系良好(r=1.0000);苯甲酸利扎曲普坦低、中、高3个浓度的平均回收率(n=3)分别为100.0%(RSD=0.96%),100.8%(RSD=1.3%),102.6%(RSD=1.5%)。结论:所建方法专属性强、准确、简便,可用于苯甲酸利扎曲普坦含量和有关物质的同时测定,且可通过对痕量杂质的检查识别失控的生产过程。
OBJECTIVE: To establish a RP-HPLC ion-pair gradient elution method for simultaneous determination of rizatriptan benzoate content and related substances. Methods: The chromatographic column was Phenomenex C18 (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-5 mmol.L-1 heptane sulfonate solution (24:76, acetic acid, pH 3.4) Phase acetonitrile-5mmol.L-1 heptane sulfonate solution (38:62, acetic acid pH3.4), gradient elution; flow rate: 1.0 mL.min-1; nm. Results: The separation of rizatriptan peak from adjacent impurities was satisfactory. Rizatriptan benzoate showed good linearity (r = 1.0000) in the range of 0.02 ~ 16μg.mL-1; The average recoveries (RSD = 0.96%), 100.8% (RSD = 1.3%), and 102.6% (RSD = 1.5%) of the three concentrations of low, medium and high concentrations of etoposide were 100.0% (n = 3) Conclusion: The proposed method is specific, accurate and convenient. It can be used for simultaneous determination of rizatriptan benzoate content and related substances, and can identify uncontrolled production process by checking trace impurities.