HPLC测定拉洛他赛中醋酸残留量检测方法的建立与验证

Establishment and Validation of HPLC Method for Determination of Acetic Acid Residue in Lalotasel

建立用外标法采用HPLC测定拉洛他赛原料中醋酸残留量的方法,并对其进行方法学验证。用Agilent TC-C_(18)色谱柱,以流动相A为0.07%磷酸溶液-甲醇(950∶50),流动相B为甲醇,等度洗脱,流速为1.0 mL/min,柱温为35℃,检测波长为210 nm。醋酸在4.0240~100.6000μg/mL浓度范围内呈良好的线性关系(r=0.9999),醋酸平均回收率(n=9)为99.5%,RSD为1.13%。经方法学验证证明所建方法简便、灵敏、准确性高、重复性好且可靠,可以有效控制拉洛他赛原料中醋酸残留量。

A method for the determination of acetic acid residue in raw materials of lalotaser by HPLC with external standard method was established,and its methodology was verified.Using Agilent TC-C_(18)chromatographic column,the mobile phase A was 0.07%phosphoric acid solution methanol(950∶50),and the mobile phase B was methanol.The flow rate was 1.0 mL/min,the column temperature was 35℃,and the detection wavelength was 210 nm.There was a good linear relationship in the concentration range of 4.0240~100.6000μg/mL of acetic acid(r=0.9999).The average recovery of acetic acid(n=9)was 99.5%and RSD was 1.13%.The method was proved to be simple,sensitive,accurate,reproducible and reliable,and can effectively control the residue of acetic acid in the raw material of lalotasal.