Sample preparation and antibiotic quantification in vinasse generated from sugarcane ethanol fuel production

Josiel José da Silva; Bianca Ferreira da Silva; Maria Valnice Boldrin Zanoni; Nelson Ramos Stradiotto

doi:10.1016/j.chroma.2022.462833

Sample preparation and antibiotic quantification in vinasse generated from sugarcane ethanol fuel production

J Chromatogr A. 2022 Mar 15:1666:462833. doi: 10.1016/j.chroma.2022.462833. Epub 2022 Jan 29.

Authors

Josiel José da Silva¹, Bianca Ferreira da Silva², Maria Valnice Boldrin Zanoni², Nelson Ramos Stradiotto³

Affiliations

¹ São Paulo State University (Unesp), Institute of Chemistry, 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil. Electronic address: josiel.silva@unesp.br.
² São Paulo State University (Unesp), Institute of Chemistry, 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil.
³ São Paulo State University (Unesp), Institute of Chemistry, 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil; São Paulo State University (Unesp), Bioenergy Research Institute (IPBEN), 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil.

PMID: 35124357
DOI: 10.1016/j.chroma.2022.462833

Abstract

Vinasse - liquid organic residue derived from the production of sugarcane ethanol fuel, has been applied as soil amendment via fertigation for decades in Brazil. This organic residue is an important source of nutrients and water for sugarcane crops. Through fertigation, approximately 400 billion liters of vinasse are recycled annually. Despite the economic and agronomic importance of this practice, vinasse-based fertigation can be a source of antibiotic contamination in the environment. The present work reports the application of solid phase extraction (SPE), salting-out liquid-liquid extraction (SALLE), and on-line solid phase extraction (on-line SPE) as sample preparation techniques for the analysis of the following antibiotics (contaminants) in vinasse sample: monensin, penicillin G, virginiamycin M1, virginiamycin S1, tetracycline and erythromycin. The study also employed a totally automated quantitative method based on on-line SPE and liquid chromatography coupled to quadrupole linear ion trap tandem mass spectrometry (LC-QqLIT-MS/MS) for the analysis of these contaminants in vinasse. The application of the aforementioned sample preparation techniques led to the successful extraction of the analytes, and a comparative analysis of the techniques showed that the on-line SPE technique was the most advantageous among the techniques investigated. The quantitative analytical method applied yielded well-defined chromatographic peaks, working range of 1.0-370.0 ng·mL^-1, apparent recovery ranging from 80 to 110% for most compounds, repeatability between 3 and 16%, and limits of detection ranging from1.0 to 10 ng·mL^-1. The analysis of six vinasse samples from different ethanol producing plants led to the detection of monensin at the concentration of 14.3 ng·mL^-1 in their compositions. The results obtained show that fertigation with vinasse is a source of antibiotic contamination in the environment.

Keywords: Antibiotic contamination; Fertigation; On-line SPE; SPE; Salting-out liquid-liquid extraction; Vinasse.

MeSH terms

Anti-Bacterial Agents / analysis
Ethanol
Saccharum*
Solid Phase Extraction / methods
Tandem Mass Spectrometry* / methods

Substances

Anti-Bacterial Agents
Ethanol