Determination of Related Substances in Calcium Dibutyryladenosine Cyclophosphate Bulk Drug by HPLC
An HPLC method was established to determine the related substances in calcium dibutyryladenosine cyclophosphate(1)bulk drug,which were sodium 2'-O-monobutyryladenosine cyclophosphate(3),sodium N6-monobutyryladenosine cyclophosphate(4)and adenosine cyclophosphate(5).The ODS Hypersil column(4.6 mm×200 mm,5 μm)was used,with 0.1 mol/L potassium dihydrogen phosphate solution-methanol(600∶400)as the mobile phase.The detection wavelength was 273 nm,the column temperature was 30 ℃ and the flow rate was 1.0 mL/min.A main component self-compare with correction factor method was established to determine three known impurities,and the correction factors of impurities 3,4,and 5 to the principal component were determined to be 1.7,0.9,and 1.4,respectively.The results showed that it was linear for sodium dibutyryladenosine cyclophosphate(2),3,4,5 in the ranges of 0.1-20,4-20,1-20,0.1-2 μg/mL,respectively.The average recoveries(n=2)of 3,4 and 5 were 101.0％,98.5％,and 99.7％,respectively,and the precision RSDs(n=6)were 0.1％,0.2％,and 0.1％,respectively.The repeatability RSDs(n=6)were 1.5％,1.6％,and 2.5％,respectively.The detection limits for 3,4,5,and 1 were 0.2,0.1,0.1,and 0.2 ng,respectively.This method has good specificity,accuracy,and sensitivity,which can provide a reference for quality research of 1.
calcium dibutyryladenosine cyclophosphateHPLCrelated substancemain component self-compare with correction factor method
万方数据
维普
