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The use of ultra-high-pressure-liquid-chromatography tandem time-of-flight mass spectrometry as a confirmatory method in drug residue analysis: Application to the determination of antibiotics in piglet liver.
Journal of Chromatography B ( IF 3 ) Pub Date : 2020-07-13 , DOI: 10.1016/j.jchromb.2020.122264
Daniela Magalhães 1 , Andreia Freitas 2 , Ana Sofia Vila Pouca 3 , Jorge Barbosa 2 , Fernando Ramos 4
Affiliation  

Consumption of food containing antibiotic residues can cause direct toxic effects, such as allergic reactions, or indirect effects, like the possibility to contribute to the development of antimicrobial resistance. It is essential for consumer food safety, as well as for public health, to monitor antibiotics in foods of animal origin intended for human consumption, particularly in piglets, a highly consumed meat in Portugal. Concerning the lack of regulations regarding the validation criteria for the ToF-MS (time-of-flight mass spectrometry) drug residues determination, this study presents an approach for the use of UHPLC (ultra-high-pressure-liquid-chromatography)-ToF-MS not only for screening but also for confirmatory purposes of 45 antibiotics from 7 different classes. Thus, a method was optimized and validated in accordance with Decision 2002/657/EC by evaluating CCα, CCβ, specificity, selectivity, recovery, ruggedness, repeatability and reproducibility. For antibiotics with no MRL set, the lowest values achieved for CCα and CCβ were, respectively, of 0.1 μg kg−1 and 0.2 μg kg−1 for cinoxacin. Regarding precision, the CV values obtained ranged from 5% to 21% for repeatability and from 6% to 22% for reproducibility. Recoveries were calculated falling between 82% and 120%. After validation, the method was used to analyse piglet liver samples. Antibiotic residues were determined in 47% of the 21 analysed samples. Nevertheless, all the antibiotics were detected at concentrations below the MRLs.



中文翻译:

超高压液相色谱串联飞行时间质谱法在药物残留分析中的确认方法:在仔猪肝中抗生素的测定中的应用。

食用含有抗生素残留物的食物会引起直接的毒性作用,例如变态反应或间接作用,例如可能导致产生抗药性。对消费者食品安全以及公共卫生至关重要的是,监测供人类食用的动物源性食品中的抗生素,尤其是在仔猪(葡萄牙的高消费肉类)中。关于缺乏有关ToF-MS(飞行时间质谱)药物残留测定验证标准的法规,本研究提出了一种使用UHPLC(超高压液相色谱)-ToF的方法-MS不仅用于筛查,还用于确认目的,共来自7个不同类别的45种抗生素。从而,通过评估CCα,CCβ,特异性,选择性,回收率,耐用性,可重复性和可重复性,根据Decision 2002/657 / EC对方法进行了优化和验证。对于未设定MRL的抗生素,CCα和CCβ的最低值分别为0.1μgkgcinoxacin -1和0.2μgkg -1。关于精度,获得的CV值的可重复性范围为5%至21%,再现性的范围为6%至22%。计算的回收率介于82%和120%之间。验证后,该方法用于分析仔猪肝脏样品。在21个分析样品中有47%确定了抗生素残留。尽管如此,所有抗生素的检出浓度均低于最大残留限量。

更新日期:2020-07-29
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