São Paulo State University (Unesp), Institute of Chemistry, 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil.
São Paulo State University (Unesp), Institute of Chemistry, 55 Prof. Francisco Degni St, Araraquara, São Paulo 14800-060, Brazil.
J Chromatogr A. 2022 Mar 15;1666:462833. doi: 10.1016/j.chroma.2022.462833. Epub 2022 Jan 29.
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, 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. 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 in their compositions. The results obtained show that fertigation with vinasse is a source of antibiotic contamination in the environment.
酒糟——从甘蔗乙醇燃料生产中获得的液态有机残渣，已通过灌溉施肥在巴西应用了几十年，作为土壤改良剂。这种有机残渣是甘蔗作物养分和水分的重要来源。通过灌溉施肥，每年约有 4000 亿升酒糟得到回收利用。尽管这种做法具有经济和农业重要性，但酒糟基灌溉施肥可能成为环境中抗生素污染的来源。本工作报道了固相萃取 (SPE)、盐析液-液萃取 (SALLE) 和在线固相萃取 (在线 SPE) 作为分析酒糟样品中以下抗生素（污染物）的样品制备技术：莫能菌素、青霉素 G、维吉尼亚霉素 M1、维吉尼亚霉素 S1、四环素和红霉素。该研究还采用了一种完全自动化的定量方法，基于在线 SPE 和液相色谱与四极线性离子阱串联质谱 (LC-QqLIT-MS/MS)，用于分析酒糟中的这些污染物。上述样品制备技术的应用成功地提取了分析物，并对技术进行了比较分析，结果表明在线 SPE 技术是所研究技术中最有利的技术。所应用的定量分析方法产生了定义良好的色谱峰，工作范围为 1.0-370.0ng·mL，大多数化合物的表观回收率在 80-110%之间，重复性在 3-16%之间，检测限在 1.0-10ng·mL 之间。对来自不同乙醇生产厂的六个酒糟样品的分析导致在其成分中检测到莫能菌素的浓度为 14.3ng·mL。所得结果表明，酒糟灌溉施肥是环境中抗生素污染的一个来源。
