Rapid determination of 12 antibiotics and caffeine in sewage and bioreactor effluent by online column-switching liquid chromatography/tandem mass spectrometry

Author(s)

Lima Gomes, Paulo C. F. ^{[1, 2]} ; Tomita, Ins N. ^[2] ; Santos-Neto, Alvaro J. ^[3] ; Zaiat, Marcelo ^[2]

Affiliation

^[1] Sao Paulo State Univ UNESP, Inst Chem, Dept Analyt Chem, BR-14800060 Araraquara, SP - Brazil

^[2] Univ Sao Paulo, Sao Carlos Sch Engn EESC, Ctr Res Dev & Innovat Environm Engn, Environm Engn, Biol Proc Lab, BR-13563120 Sao Carlos, SP - Brazil

^[3] Univ Sao Paulo, Inst Chem Sao Carlos, BR-13560970 Sao Carlos, SP - Brazil

• Document type: Journal article
• Source: ANALYTICAL AND BIOANALYTICAL CHEMISTRY; v. 407, n. 29, p. 8787-8801, NOV 2015.
• Web of Science Citations: 11

Abstract

This study presents a column-switching solid-phase extraction online-coupled to a liquid chromatography/tandem mass spectrometry (SPE-LC-MS/MS) method for simultaneous analysis of 12 antibiotics (7 sulfonamides and 5 fluoroquinolones) and caffeine detected in the sewage and effluent of a pilot anaerobic reactor used in sewage treatment. After acidification and filtration, the samples were directly injected into a simple and conventional LC system. Backflush and foreflush modes were compared based on the theoretical plates and peak asymmetry observed. The method was tested in terms of detection (MDL) and quantification limit (MQL), linearity, relative recovery, and precision intra- and inter-day in lab-made sewage samples. The method presented suitable figures of merit in terms of detection, varying from 8.00 x 10(-5) to 6.00 x 10(-2) ng (0.800 up to 600 ng L-1; caffeine) with direct injection volume of only 100 mu L and 13 min of total analysis time (sample preparation and chromatographic run). When the method was applied in the analysis of sewage and effluent of the anaerobic reactor (n = 15), six antibiotics and caffeine were detected in concentrations ranging from 0.018 to 1097 mu g L-1. To guarantee a reliable quantification, standard addition was used to overcome the matrix effect. (AU)

• FAPESP's process: 09/15984-0 - Bioenergy production from wastewaters and environmental fitting of liquid and solid wastes generated
• Grantee: Marcelo Zaiat
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 10/19910-9 - Development of green chemistry strategies on chromatography and application to the evaluation of antibiotics degradation in wastewaters by fixed-bed anaerobic bioreactors
• Grantee: Alvaro José dos Santos Neto
• Support Opportunities: Regular Research Grants
• FAPESP's process: 12/07153-4 - Analysis and identification of degradation products of antibiotics after treatment in anaerobic reactors
• Grantee: Paulo Clairmont Feitosa de Lima Gomes
• Support Opportunities: Scholarships in Brazil - Post-Doctoral