RP-HPLC离子对梯度洗脱法同时测定苯甲酸利扎曲普坦含量和有关物质

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,5 μm);流动相:A相为乙腈-5 mmol·L^-1庚烷磺酸钠溶液(24∶ 76,醋酸调pH 3.4),B相为乙腈-5 mmol·L^-1庚烷磺酸钠溶液(38∶ 62,醋酸调pH 3.4),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0.02~16 μg·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 an HPLC method for simultaneous determination of rizatriptan benzoate and its related substances. Methods: The C₁₈ column (250 mm×4.6 mm,5 μm) was used.The mobile phase consisted of two solvents,A and B with gradient elution.The A solvent was acetonitrile-5 mmol·L^-1 sodium heptanesulfonate (24∶ 76,pH 3.4 adjusted with acetic acid);the B solvent was acetonitrile-5 mmol·L^-1 sodium heptanesulfonate (38∶ 62,pH 3.4 adjusted with acetic acid).The flow rate was 1.0 mL·min^-1.The column temperature was 30 ℃.The detection wavelength was 227 nm. Results: Rizatriptan peak was successfully separated from its nearby impurity peaks.The linear range of calibration curve for rizatriptan benzoate was 0.02-16 μg·mL^-1 (r=1.0000).The average recoveries (n=3) for rizatriptan benzoate in low,middle and high concentration were 100.0% (RSD=0.96%),100.8% (RSD=1.3%),102.6% (RSD=1.5%),respectively. Conclusions: The established method is validated to be specific,accurate and simple for simultaneous determination of rizatriptan benzoate and its related substances.And it can identify out-of-control processes on the basis of trace impurity tests.