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Simultaneous extraction and determination of 45 veterinary antibiotics in swine manure by liquid chromatography-tandem mass spectrometry.
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2020-07-28 , DOI: 10.1016/j.jchromb.2020.122286
Suli Zhi 1 , Jing Zhou 2 , Haixue Liu 3 , Huihui Wu 3 , Zulin Zhang 4 , Yongzhen Ding 1 , Keqiang Zhang 1
Affiliation  

A multiresidue method for identification and quantification of 45 veterinary antibiotics (VAs) belonging to 5 different drug classes has been developed, which is the first comprehensive method for pig manure. The proposed method used mixed liquor with methanol: acetonitrile: citrate buffer ratio of 1:1:2 to extract the target VAs from freeze-dried manure. The extracting solution passed through solid-phase extraction (SPE) procedure with Oasis HLB cartridges, which could isolate the target VAs and clean the samples in a single step. After blow-drying and concentrating, the samples were analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in one single injection with a run time of 12 min. The average recovery rates for most of the VAs were in the range of 50–120% with relative standard deviations below 15%. Linearity was studied in the range between 2 and 1000 μg/kg using matrix-matched calibration and pure solvent calibration, to evaluate the matrix effects (MEs). The limits of detection (LDs) and quantification (LQs) were in the range of 0.01–1.54 μg/kg and 0.03–5.13 μg/kg respectively, except for penicillin G. Finally, the proposed method was used to quantify VA residues in real swine manure from three farms with different scales; tetracyclines, sulfonamides, quinolones and macrolides were the most frequently detected compounds.



中文翻译:

液相色谱-串联质谱法同时提取和测定猪粪中的45种兽用抗生素。

已开发出一种用于鉴定和定量5种不同药物类别的45种兽用抗生素的多残留方法,这是第一种用于猪粪的综合方法。所提出的方法使用混合液与甲醇:乙腈:柠檬酸盐的缓冲液比例为1:1:2,以从冻干肥料中提取目标VA。萃取溶液通过Oasis HLB柱通过固相萃取(SPE)程序,可以分离目标VA并在一个步骤中清洁样品。吹干并浓缩后,通过超高效液相色谱-串联质谱法(UHPLC-MS / MS)在单次进样中分析样品,运行时间为12分钟。大多数VA的平均回收率在50–120%的范围内,相对标准偏差低于15%。使用基质匹配校准和纯溶剂校准研究了线性范围为2至1000μg/ kg的线性,以评估基质效应(MEs)。除了青霉素G外,检出限(LDs)和定量限(LQs)分别在0.01–1.54μg/ kg和0.03–5.13μg/ kg范围内。最后,提出的方法用于定量分析真实的VA残留量来自三个规模不同的农场的猪粪;四环素,磺酰胺,喹诺酮和大环内酯类化合物是最常检测到的化合物。该方法用于量化三个规模不同的猪场中真实猪粪中的VA残留量。四环素,磺酰胺,喹诺酮和大环内酯类化合物是最常检测到的化合物。该方法用于量化三个规模不同的猪场中真实猪粪中的VA残留量。四环素,磺酰胺,喹诺酮和大环内酯类化合物是最常检测到的化合物。

更新日期:2020-08-02
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