Chen Jian-dong, Chen Jian-yang, Zhang Lin-hai
2015
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Journal
Chinese Journal of Pharmaceutical Analysis
Abstract
Objective: To develop a high performance liquid chromatographic method with fluorimetric detection after precolumn derivatization with fluorescamine for 3- chloro-4-( 3- fluorobenzyloxy)- aniline( hereinafter called genotoxic impurity) determination in lapatinib ditosylate. Methods: The 3-chloro-4-( 3-fluorobenzyloxy)-aniline in lapatinib ditosylate was derived with fluorescamine at p H 3. 3,and analyzed by high performance liquid chromatography equipped with fluorescence detector. The Kromasil 100-5C18column( 150 mm × 4. 6 mm,5 μm) was adopted for the analysis with a mobile phase consisting of 0. 05 mol·L-1aqueous ammonium acetate( p H 4. 5) and acetonitrile( 50∶ 50) at the flow rate of 1. 3 m L·min-1,and the fluorescence detection was set λex= 290 nm and λem= 503 nm. Results: The calibration curve was linear over the concentration range from 5 ng·m L-1to 50 ng·m L-1with the correlation coefficient of 0. 996 1; the limit of quantity was 2. 0 ng·m L-1( equal to 0. 000 04%),the average recovery( n = 12) was 96. 4%. The results of three batchs of samples were 0. 000 10%,0. 000 08% and 0. 00011%,respectively. Conclusion: The established method is proved to be suitable for the determination of 3-chloro-4-( 3-fluorobenzyloxy)-aniline in lapatinib ditosylate.