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Quantification of multi-class antibiotics by UHPLC-MS/MS analysis combined with salt-assisted acetonitrile extraction: comparative evaluation of dairy and poultry manure

机译:通过UHPLC-MS / MS分析与盐辅助乙腈萃取相结合的多类抗生素定量:奶牛和家禽粪便的比较评估

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A comprehensive multiresidue method for the analysis of 33 antibiotics from 7 prevalent classes was comparably investigated for both dairy and poultry manure samples, which can be important pollution sources for the release of antibiotics into the environment. Following salting-out-assisted extraction with acetonitrile, the antibiotics were quantified with ultrahigh-performance liquid chromatography tandem mass spectrometry without a clean-up step. By changing the composition of the mobile phase for chromatography, a pronounced signal enhancement was achieved not only for tetracyclines (TCs) but also for other groups of antibiotics in the manure samples. Although the physicochemical properties of selected antibiotics were quite different, the apparent recovery values from dairy and poultry manure samples by using an extraction solvent comprising McIlvaine buffer and ethylenediaminetetraacetic solution at pH 3 were 86-121% and 89-113%, respectively. Apparent recovery of the antibiotics was not remarkably affected by the extraction solvent over a wide range of pH values, with the exception of the recovery of TC antibiotics from poultry manure, which was in the 53-55% range at pH 8. Furthermore, the poor performance of the analytical method for a few of the antibiotics in poultry manure was correlated with high metal and organic contents of the complicated matrix. The high suppression effects of co-eluted matrix components were compensated by constructing matrix-matched calibration curves and by using internal standards. Simultaneous quantification of seven different antibiotic classes with low limit of detection values varying from 0.38 to 31 mu g kg(-1) for dairy manure and from 0.32 to 5.85 mu g kg(-1) for poultry manure facilitated their monitoring. The application of the developed analytical method to dairy, broiler and layer-hen manure samples from confined animal feeding operations showed that a wide variety of antibiotics at high concentrations were found in broiler manure.
机译:比较了分析奶牛和家禽粪便样品中7种流行类别中33种抗生素的综合多残留方法,这可能是释放抗生素到环境中的重要污染源。用乙腈盐析辅助萃取后,无需清洗即可通过超高效液相色谱串联质谱法对抗生素进行定量。通过改变色谱中流动相的组成,不仅对四环素(TC),而且对粪便样品中的其他抗生素组均实现了明显的信号增强。尽管所选抗生素的理化特性差异很大,但使用包含McIlvaine缓冲液和乙二胺四乙酸溶液的萃取溶剂(pH 3)从乳制品和家禽粪便样品中获得的表观回收率分别为86-121%和89-113%。在很宽的pH值范围内,提取溶剂并未明显影响抗生素的表观回收率,但从家禽粪便中回收TC抗生素的情况除外,pH值为8时,回收率在53-55%之间。家禽粪便中几种抗生素的分析方法性能不佳与复杂基质中金属和有机物含量高有关。通过构建基质匹配的校准曲线并使用内标补偿了共洗脱基质组分的高抑制效果。对7种不同的抗生素类同时进行定量,其检出限的下限范围从乳品粪便的0.38至31μg kg(-1)和家禽粪便的0.32至5.85μg kg(-1)便于监测。改进的分析方法在受限动物饲养操作中的奶制品,肉鸡和蛋鸡粪肥样品中的应用表明,在肉鸡粪中发现了多种高浓度的抗生素。

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