Reversed phase ion-pair high performance liquid chromatographic gradient separation of related impurities in 2,4-disulfonic acid benzaldehyde di-sodium salt.
A reversed phase ion-pair gradient liquid chromatographic method has been developed and validated for purity determination of the hydrophilic compound 2,4-disulfonic acid benzaldehyde di-sodium salt (2,4-DSAD) containing both hydrophilic and more lipophilic related impurities. Mixtures of acetonitrile-phosphate buffer containing tetrahexylammonium hydrogen sulfate as the ion-pairing reagent were used as the mobile phase. A linear gradient, which generated simultaneous change in the concentration of organic modifier, buffer concentration and the concentration of ion-pairing reagent, was applied. The method allows detection of impurities at low levels (0.01% w/w). Excellent repeatability for both retention time (RSD< or =0.3%, n = 6) and detector response (RSD = 0.03%, n = 6 for the main peak and RSD = 6%, n = 6, for an impurity at 0.01 area% level) was obtained. The method was shown to be robust for routine analysis and has been successfully transferred to the quality control laboratory.
Lu
Bing
B
Analytical Chemistry, Process R&D, AstraZenca R&D, Södertälje, Sweden. bing.lu@astrazeneca.com
Jonsson
Peter
P
Blomberg
Sverker
S
D000097:Acetonitriles; D001547:Benzaldehydes / Q000302:isolation & purification*; D001557:Benzenesulfonates / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013696:Temperature
C513225:2,4-disulfonic acid benzaldehyde; D000097:Acetonitriles; D001547:Benzaldehydes; D001557:Benzenesulfonates; C032159:acetonitrile