4th Annual WML Academic Symposium

Marine toxins like Okadaic acid (OA), Calyculin A and Microcystin-LR play an important role in protein phosphatase inhibition. The goal of this research is to develop GC-MS method to quantify Okadaic acid and to overcome the sensitivity found in previous studies using HPLC-MS method. Silylation reaction was chosen to derivatize OA using the derivatizing reagent MTBSTFA (1% TBDMCS as catalyst) to improve its volatility required for GC-MS analysis. Thin Layer Chromatography (TLC) was first used to monitor derivatizing reaction. The reaction mixture was also analyzed by HPLC-MS. The TLC and HPLC-MS results indicated the formation of derivative and disappearance of OA initially added to the reaction mixture. GC-MS analysis will be performed next which will comprise optimization of GC & MS parameters such Full MS or SIM. The GC-MS method will be compared with the previous study performed on the same Okadaic acid using HPLC-MS to see whether GC-MS will be more sensitive. The reported values of LOQ and correlation coefficient were 402.25pg and 0.9984 respectively in the previous study performed using HPLC-MS analysis.