摘要
采用超临界流体色谱(SFC)系统分离并测定盐酸厄洛替尼(1)及其4种有关物质.采用Torus 2-PIC柱(3.0 mm×100 mm,1.7 μm),以超临界二氧化碳-甲醇为流动相进行梯度洗脱,进样量为1 μL,柱温为50℃,流速为1.0 mL/min.结果显示,各化合物在7 min内出峰并分离完全;4种有关物质分别在0.5～40,2～60、0.4～40、0.5～40 μg/mL内,1在5～100μg/mL内,线性关系良好.1、杂质A、杂质B、杂质C和杂质D的LOD分别为0.2、0.2、0.5、0.1、0.2μg/mL;LOQ分别为0.5、0.5、2.0,0.4、0.5 μg/mL.各有关物质的加样回收率(n=3)在96.0％～104.2％,RSD均小于 3.0％.建立的方法快速有效、灵敏度高、绿色环保,可有效用于1原料药及片剂的质量控制.
Abstract
A supercritical fluid chromatography(SFC)method was established for the separation and determination of erlotinib hydrochloride(1)and its four related substances.A Torus 2-PIC column(3.0 mm×100 mm,1.7 μm)was used with the mobile phase containing a mixture of supercritical CO2 and methanol by gradient elution.The injection volume was 1 μL,the column temperature was 50 ℃,and the flow rate was 1.0 mL/min.The results showed that each compound peaked and was completely separated within 7 minutes.And it was linear for four related substances and 1 in the ranges of 0.5-40,2-60,0.4-40,0.5-40,5-100 μg/mL,respectively.The LODs of 1 and impurities A,B,C,D were 0.2,0.2,0.5,0.1,0.2 μg/mL,respectively,and the LOQs were 0.5,0.5,2.0,0.4,0.5 μg/mL,respectively.The recoveries(n=3)of four related substances were between 96.0％and 104.2％,with RSDs all less than 3.0％.The established method is rapid,effective,highly sensitive,environmentally friendly,which can be effectively used for quality control of 1 bulk drug and tablets.
维普
万方数据