Paper
SUN Zhen, XU Mingming, YAN Cuixia, ZHENG Luxia, SHAO Hong
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 ffow 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 speciffcity, accuracy, and sensitivity, which can provide a reference for quality research of 1.