Chemosphere ( IF 5.778 ) Pub Date : 2021-02-22 , DOI: 10.1016/j.chemosphere.2021.130039 Manuel Argüeso-Mata; Silvia Bolado; Juan José Jiménez; Rebeca López-Serna
The presence of residues of veterinary pharmaceuticals in farm wastewaters such as pig slurry represents a problem that needs to be tackled to avoid further contamination of environmental waters and the development of resistant bacteria. For their monitoring and control, it is necessary the existence of reliable analytical tools. The present paper describes for the first time the development and optimization by statistical experimental design of a specifically designed analytical method for the analysis of 21 veterinary drugs, including 18 antibiotics of several families (β-lactams, tetracyclines, fluoroquinolones, sulfonamides, macrolides, among others), 1 antiparasitic, 1 analgesic and 1 hormone, in a complex environmental matrix such as the fresh solid phase of pig slurry. The resulting method, consisted of an ultrasound assisted extraction (UAE) combined with in-situ dispersive solid phase extraction (d-SPE) from a 0.3 g of freeze-dried sample aliquot followed by a preconcentration step by compact solid phase extraction (c-SPE) and subsequent instrumental analysis by ultra-high-performance-liquid-chromatography (UHPLC) coupled to mass spectrometry in tandem (MS/MS) by a triple quadrupole, was successfully validated as a very sensitive (method limit of quantification in the low ng g−1) and reliable method (relative recoveries around 100% and method repeatability featured by a general relative standard deviation below 20%). Provided raw data was intended to be processed by matrix-matched quantification approach. The resulting methodology was applied to the characterization of several pig manures from different Spanish farms sampled across breeding season between 2018 and 2019. Sample precedence showed to have a high impact in the positives, its frequency and concentration.
农场废水（如猪粪）中存在兽药残留是一个需要解决的问题，以避免环境水的进一步污染和耐药细菌的产生。为了对其进行监视和控制，必须存在可靠的分析工具。本文首次通过统计实验设计描述了一种专门设计的分析方法的开发和优化，该分析方法可用于分析21种兽药，包括几种家族的18种抗生素（β-内酰胺类，四环素类，氟喹诺酮类，磺酰胺类，大环内酯类，其他），1种抗寄生虫药，1种镇痛药和1种激素，它们存在于复杂的环境基质中，例如新鲜的猪粪便固相。产生的方法，从0.3 g冻干样品等分试样中进行原位分散固相萃取（d-SPE），然后通过紧凑固相萃取（c-SPE）进行预浓缩，然后通过超高效液相色谱仪进行仪器分析三重四极杆串联质谱联用（MS / MS）色谱法（UHPLC）已被成功验证为非常灵敏（低ng g -1的定量方法极限））和可靠的方法（相对回收率在100％左右，并且方法的可重复性以低于20％的一般相对标准偏差为特征）。提供的原始数据打算通过矩阵匹配量化方法进行处理。所得方法论被用于表征2018年至2019年整个繁殖季节采样的来自西班牙不同农场的几种猪粪。样品的优先次序显示出对阳性，频率和浓度有很大影响。