METHOD DEVELOPMENT OF MACROLIDE AND PLEUROMUTILIN ANTIBIOTICS IN LIQUID MANURE SAMPLES BY LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

• Main Authors: , Juwita Ayu Manggalarini, , Dr. Roto, M.Eng.
• Format: Theses and Dissertations NonPeerReviewed
• Published: [Yogyakarta] : Universitas Gadjah Mada 2013
• Subjects: ETD
• Online Access: https://repository.ugm.ac.id/123456/; http://etd.ugm.ac.id/index.php?mod=penelitian_detail&sub=PenelitianDetail&act=view&typ=html&buku_id=63567
• Institution: Universitas Gadjah Mada

Method development for analysis of macrolide and pleuromutilin antibiotics in liquid manure samples was developed. Optimization of mass spectrometry and liquid chromatography separation for the target compounds was firstly conducted following with development of the clean-up procedure using solid phase extraction (SPE). Three methods to extract the target compounds in the liquid manure samples were checked. Ultrasound and centrifugation assisted extraction, then direct solvent extraction and the next extraction was lyophilization and solvent extraction. Urea and 5% of EDTA as additives were also used to optimize the extraction efficiencies in the direct solvent extraction and lyophilization and solvent extraction. The results showed that Zorbax Eclipse Plus C18 column was suitable for separation of macrolide and pleuromutilin antibiotics. Liquid chromatography tandem mass spectrometry (LC/MS/MS) using electrospray ionization in positive mode (ESI+) was used for detection of the target compounds. Testing for the SPE cartridges was performed using hydrophilic lipophilic balance (60-mg HLB), weak cationic exchange (200-mg WCX), mixed of reversed-phase cation exchange (60-mg MCX), C18 (1000-mg) and C18 polar plus (1000-mg). All of the extraction methods gave poor recoveries of the target compounds, except for lyophilization and solvent extraction using citric acid buffer (pH 4.7) with addition of urea and using phosphate buffer (pH 9.0) with addition of 5% EDTA.