Trace level detection and quantitation of ethyl diazoacetate by reversed-phase high performance liquid chromatography and UV detection.
A method using reversed-phase high performance liquid chromatography (HPLC) with UV detection has been developed and validated for the trace level (ng/mL) detection and quantitation of ethyl diazoacetate (EDA), a toxic impurity, in sample matrix. Method development included the evaluation of several analytical techniques including LC-MS and GC-MS, which in this case, proved to be unacceptable means of analysis. The chromatographic separation employed in this method utilizes a mobile phase system of acetonitrile and water with analysis carried out using UV detection at 250 nm. The final method showed excellent linearity, accuracy, repeatability, specificity and recovery when evaluated at the quantitation limit (QL) of 6 ng/mL.
Axe
Brian P
BP
Analytical Sciences Research & Development, Eli Lilly & Company, Lilly Corporate Center, Indianapolis, IN 46285, USA. axe_brian_p@lilly.com
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003979:Diazonium Compounds / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*
D003979:Diazonium Compounds; C032111:diazoacetic ester