Preparative counter-current chromatography purification of valrubicin (AD-32) from crude synthetic drug using upright coil planet centrifuge with four multilayer coils connected in series.
Preparative counter-current chromatography (CCC) purification of valrubicin (AD-32) from crude synthetic drug has been successfully performed for the first time using upright coil planet centrifuge with four multilayer coils connected in series with 1600 ml capacity. The two-phase system used was composed of light petroleum (bp 60-90 degrees C)-ethyl acetate-tetrachloromethane-methanol-water at an optimized volume ratio of 1:1:8:6:1. Target compound (1.2 g) with a purity of 99.88% was obtained from 1.5 g of crude synthetic drug with a purity 95.49% based on HPLC peak area percentage. Identification of the target compound was performed by electrospray ionization mass spectrometry, one- and two-dimensional nuclear magnetic resonance.
Wu
Shihua
S
Zhejiang University, College of Life Sciences, Hangzhou 310058, China.
Sun
Cuirong
C
Pan
Yuanjiang
Y
D002498:Centrifugation / Q000295:instrumentation* / Q000379:methods; D003377:Countercurrent Distribution / Q000379:methods*; D004317:Doxorubicin / Q000031:analogs & derivatives* / Q000302:isolation & purification; D021241:Spectrometry, Mass, Electrospray Ionization
C016163:valrubicin; D004317:Doxorubicin