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

Balaji Nagarajan * and Gunasekar Manoharan2

New Jersey Bioscience Centre, 685, North Brunswick, New Jersey, United States of America.
 
Research Article
International Journal of Scholarly Research in Chemistry and Pharmacy, 2023, 02(02), 001–007.
Article DOI: 10.56781/ijsrcp.2023.2.2.0019
Publication history: 
Received on 09 May 2023; revised on 19 June 2023; accepted on 22 June 2023
 
Abstract: 
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%.
 
Keywords: 
EIBA; GC; GC-MS; Validation; Impurities; Stress study
 
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