METHOD DEVELOPMENT FOR THE DETERMINATION OF IMAZALIL AND ITS METABOLITES IN WATER SAMPLES USING SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY � TANDEM MASS SPECTROMETRY

• Main Authors: , Arum Widyasari, , Prof. Dr. Endang Tri Wahyuni, M.S.
• Format: Theses and Dissertations NonPeerReviewed
• Published: [Yogyakarta] : Universitas Gadjah Mada 2011
• Subjects: ETD
• Online Access: https://repository.ugm.ac.id/90128/; http://etd.ugm.ac.id/index.php?mod=penelitian_detail&sub=PenelitianDetail&act=view&typ=html&buku_id=52450
• Institution: Universitas Gadjah Mada

In this work, a sensitive and selective method for the determination of imazalil and its 5 selected metabolites in water samples using solid phase extraction (SPE) and liquid chromatography � tandem mass spectrometry (LC-MS/MS) has been developed. Three water matrices were used, i.e., deionised, surface and waste water. The extraction efficiencies of OASIS HLB, OASIS MCX, Strata X, C18 and C18 polar plus cartridges were checked in acidic condition. OASIS HLB was then chosen for further experiments due to the highest recoveries for all target compounds, yielded 97% to 101%. The performance of analytical instruments, i.e., high performance liquid chromatography-diode array detector (HPLC-DAD) and LC-MS/MS, to determine the target compounds were compared as well using fortification experiments. Results showed that LC-MS/MS detection gave higher sensitivity and selectivity for all target compounds in comparison with HPLC-DAD. The value of method detection limit (MDL) and method quantification limit (MQL) for both methods are at concentration of µg L -1 and ng L -1 for HPLC-DAD and LC-MS/MS, respectively. The evaluation of matrix effects from surface water samples analysed by SPE and LC- MS/MS showed there was an ion suppression phenomenon at low values, -1% to -7%, and thus, it could be neglected. The validation results of SPE and LC-MS/MS method consistently demonstrated the accuracy and precision to meet the acceptance criteria, the accuracy range, -30% to +20%, and the precision value � 20%. In addition, the applicability of SPE and LC-MS/MS method for screening analysis or identification of the target compounds was achieved in this work. Imazalil was found in all investigated waste water samples from waste water treatment plant (WWTP) Weddel and Steinhof, Germany, both influent and effluent at very low concentration, below the MQL of imazalil.