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采用固相萃取技术从完整牛奶中提取选定的青霉素类抗生素残留,然后用高效液相色谱法和二极管阵列检测法进行检测。

Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.

Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.

出版信息

Food Chem. 2017 Jun 1;224:131-138. doi: 10.1016/j.foodchem.2016.12.024. Epub 2016 Dec 15.

DOI:10.1016/j.foodchem.2016.12.024
PMID:28159247
Abstract

Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation.

摘要

纤维增强相固相萃取(FPSE)是一种新型的基于吸附剂的微萃取方法,被评估为一种从牛奶中提取四种青霉素抗生素残留(苄青霉素、氯唑西林、双氯西林和苯唑西林)的简单快速策略,无需预先进行蛋白质沉淀。成功地从样品制备工作流程中省去了耗时的溶剂蒸发和再构成步骤。FPSE 利用柔性纤维基底,化学涂覆溶胶-凝胶衍生的高效有机-无机杂化吸附剂作为萃取介质。在此,短链聚乙二醇(PEG)为所选青霉素提供了最佳的萃取灵敏度,采用反相高效液相色谱法(RP-HPLC)进行分析,并根据欧洲 657/2002/EC 号决定进行了验证。苄青霉素的定量限为 10μg/kg,氯唑西林为 20μg/kg,双氯西林为 25μg/kg,苯唑西林为 30μg/kg。这些与文献报道的数量级相似,并且(除了苄青霉素)均低于欧洲法规设定的最大残留限量(MRL)。

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