GC-FID and GC-MS detection of Ethyl Isobutyryl Acetate as regulatory starting material

We developed GC-FID and GC-MS methods to determine the assay and chromatographic purity of Ethyl isobutyryl acetate (EIBA). The symmetric peak shape was on a DB-Wax stationary phase with the dimensions of 30 m column length, 0.25 mm as internal diameter, 0.50 microns film thickness with the mobile phase as helium gas in temperature ramping mode at a flow rate of 1.5 mL/min using flame ionization detector and mass spectrometer. The USP resolution between EIBA and its unknown impurities was more than 2.0, indicating a significant separation. Regression analysis shows a correlation coefficient greater than 0.999 for EIBA assay and chromatographic purity techniques. The detection and quantitation limits of EIBA are 0.01% and 0.03% for the chromatographic purity procedure. This method indicates that the recovery at different levels is 90 to 110% accurate. The test solution was stable in the diluent for 48 h and subjected to stress conditions. The mass balance was close to 99.5%.