梯度洗脱HPLC法测定尼莫地平原料药中残留醋酸

Determination of residual acetic acid in nimodipine by gradient elution HPLC

目的建立高效液相色谱法测定尼莫地平原料药中残留溶剂-醋酸的方法.方法采用反相梯度洗脱高效液相色谱法,色谱柱为Welch Materials XB-C18(4.6 mm×250 mm,5μm);流动相A为每1 000 mL水含磷酸0.7 mL的溶液(调pH 3.0),流动相B为甲醇;流速为1.2 mL·min-1;检测器采用紫外检测器,波长为210 nm.结果日内精密度RSD=0.28%;平均加样回收率为98.8%(RSD=0.34%,n=9);醋酸的浓度在5.07～202.8μg·mL-1的范围内线性关系良好,相关系数r=0.999 9;方法的检测限为1.0μg·mL-1,定量限为5.0μg·mL-1.结论本方法结果准确,精密度好、灵敏度高,适用于尼莫地平原料药中残留醋酸的分析检测.

Objective To establish an HPLC method for the determination of residual acetic acid in nimodipine.Methods The RP-HPLC and gradient elution method was adopted on Welch Materials XB-C18（4.6 mm×250 mm,5 μm）column with a solution of 1 000 mL water and 0.7 mL phosphoric acid（adjusted pH 3.0 with NaOH）as mobile phase A and methanol as mobile phase B.The flow rate was 1.2 mL·min-1.The detection wavelength was 210 nm.Results The RSD of with-day precision was 0.28%,the average recovery was 98.8%（RSD=0.34%,n=9）.The linear range of acetic acid was 5.07~202.8 μg·mL-1（r=0.999 9）.The limit of detection was 1.0 μg·mL-1 and the limit of quantification was 5.0 μg·mL-1.Conclusion The method was accurate with high sensitivity and precision,and it was suitable for the determination of residual acetic acid contained in nimodipine.