Establishment of HPLC Method for Determination of 7 Main Related Substances in Tolasemide Tablets
Objective To establish a HPLC method for the determination of 7 main related substances in torasemide tablets.Methods Two major impurities F and G,which have not yet been established as standard,were separated from the API and the structure was confirmed by 1H-NMR.On this basis,the impurity content of A,B,C,D,E,F,G in torasemide tablets was determiened by HPLC.An HPLC method was adopted with ACE C18 column(100 mm× 4.6 mm,3 μm);the mobile phase was 0.02 mol/L KDP(phosphoric acid adjusted pH to 3.5)-methanol,gradient elution.The flow rate was 0.8 mL/min;the column temperature was 30 ℃;the detection wavelength is 288 nm;the injection volume was 20 μL.Results Under this chromatographic condition,7 impurities can be detected at the same time,and each impurity was well separated from torasemide,and the separation degree was greater than 1.5.The limits of quantitation were 0.083 5,0.009 9,0.020 4,0.084 3,0.024 3,0.025 5,0.039 8 μg/mL;the limits of detection were 0.025 1,0.003 9,0.006 1,0.025 3,0.007 3,0.007 7,0.012 0 μg/mL.The linear ranges of them were 0.334 0-1.336 0,0.794 6-3.178 2,0.326 4-1.305 6,0.337 2-1.348 8,0.323 8-1.295 0,0.430 3-1.021 0,0.3187-0.9561 μg/mL.The solution stability of the impurities was good within 48 h,and the RSD of the peak area was less than 3.0％(n=7).The average recovery of low,medium and high recovery solutions was 90.6％～106.6％(n=3).Conclusion This study improved the quality control method of torasemi tablets and the method is simple,sensitive,reproducible and durable,and can be used for the quality control of quetiapine fumarate tablets.
万方数据
维普
