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猪肾、肝和肺中莱克多巴胺分析:使用 QuEChERS 作为样品前处理步骤扩展方法范围的验证。

Ractopamine analysis in pig kidney, liver and lungs: A validation of the method scope extension using QuEChERS as a sample preparation step.

机构信息

Embrapa Suínos e Aves, BR 153, km 110, 89715-899 Concórdia/SC, Brazil.

Escola Superior de Agricultura Luiz de Queiroz, USP/Esalq, Av. Pádua Dias 11, 13418-900 Piracicaba/SP, Brazil.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 1;1091:79-86. doi: 10.1016/j.jchromb.2018.05.033. Epub 2018 May 23.

DOI:10.1016/j.jchromb.2018.05.033
PMID:29852384
Abstract

Ractopamine has been allowed by some countries as a repartitioning additive in pig diet, since it promotes protein synthesis and fat lipolysis. Most regulatory agencies only propose the ractopamine assessment in meat, kidney, liver and fat. Aiming at contributing to the scarcity data regarding this analyte in pig lungs, we extended the scope of a LC-MS method to evaluate pig offals. Homogenized tissue samples were extracted by a QuEChERS procedure; following by clean up steps and further tandem mass spectrometry determination. Method performance was evaluated through specificity, recovery, linearity, reproducibility, repeatability, decision limit (CC), and detection capability (CC), in accordance to the Commission Decision 2002/657/EC. Regression coefficients (R) between 0.994 and 0.999 were achieved for kidney, liver and lungs. Recoveries ranged from 92.0 to 127%. CC and CC values ranged from 3.65 to 4.86 μg kg, and from 6.27 to 7.21 μg kg, respectively. These values were under the maximum residue limits suggested by Codex Alimentarius, which are 90 and 40 μg kg for kidney and liver, respectively. When applied to real samples up to 22.5, 92 and 1003 μg kg of ractopamine residues were detected in pig liver, kidney and lungs, respectively. The results allowed concluding that the proposed analytical method is capable to detect ractopamine residues in all evaluated matrices. Therefore, it can be successfully applied and used as a routine method in laboratories of residue analysis.

摘要

莱克多巴胺已被一些国家允许作为猪饲料中的再分配添加剂,因为它能促进蛋白质合成和脂肪分解。大多数监管机构仅建议在肉、肾脏、肝脏和脂肪中评估莱克多巴胺。为了补充关于猪肺中这种分析物的稀缺数据,我们扩展了 LC-MS 方法的范围,以评估猪内脏。将组织样品均质化后,采用 QuEChERS 程序提取;然后进行净化步骤和串联质谱测定。方法性能通过特异性、回收率、线性、重现性、重复性、决策限 (CC) 和检测能力 (CC) 进行评估,符合委员会 2002/657/EC 号决定。肾脏、肝脏和肺的回归系数 (R) 分别在 0.994 到 0.999 之间。回收率在 92.0%到 127%之间。CC 和 CC 值分别在 3.65 到 4.86μg/kg 和 6.27 到 7.21μg/kg 之间。这些值低于食品法典委员会建议的最大残留限量,分别为肾脏和肝脏的 90 和 40μg/kg。当应用于实际样品时,在猪肝脏、肾脏和肺中分别检测到 22.5、92 和 1003μg/kg 的莱克多巴胺残留。结果表明,所提出的分析方法能够检测所有评估基质中的莱克多巴胺残留。因此,它可以成功地应用于残留分析实验室,并作为常规方法使用。

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