Determination of Related Substances in N-tert-Butoxycarbonyl-5,7-dichloro-1,2,3,4-tetrahydroisoquinoline-6-carboxylic Acid by HPLC
An HPLC method was established to determine the related substances in N-tert-butoxycarbonyl-5,7-dichloro-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid(1),a key starting material for lifitegrast.A Thermo Acclaim™Mixed-Mode WAX-1 column(4.6 mm×250 mm,5 μm)was used,and the analysis was carried out in the gradient elution mode with 30 mmol/L potassium dihydrogen phosphate solution-acetonitrile(95∶5)as mobile phase A,and acetonitrile-tetrahydrofuran(80∶20)as mobile phase B.The flow rate was 0.9 mL/min,the column temperature was 30 ℃,the detection wavelength was 205 nm,and the injection amount was 50 μL.The results showed that the separation between the main component and various impurities was good,and it was linear for the main component and various impurities in the corresponding concentration ranges.The average recoveries(n=9)were 96.4％-105.6％,with the RSDs less than 5.1％.This method is easy to operate,accurate,and reliable,which is suitable for the determination of related substances in1.
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