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

Ion-pair RP-HPLC simultaneous determination in gradient elution mode of rizatriptan benzoate and its related substances

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 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.