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液相色谱中的核壳结构:在使用传统色谱系统测定饲料和肉类中磺胺类药物的应用

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems.

作者信息

Armentano Antonio, Summa Simona, Magro Sonia Lo, D'Antini Pasquale, Palermo Carmen, Muscarella Marilena

机构信息

Pharmacology and Toxicology Unit, Complex Structure of Chemistry, Institute for Experimental Veterinary Medicine of Apulia and Basilicata , Foggia, Italy.

Department of Agricultural, Food, and Environmental Sciences, University of Foggia , Foggia, Italy.

出版信息

Ital J Food Saf. 2016 Dec 6;5(4):6166. doi: 10.4081/ijfs.2016.6166. eCollection 2016 Sep 20.

Abstract

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster.

摘要

采用填充有核壳颗粒的C18柱,通过配备二极管阵列检测器的传统高效液相色谱系统对饲料和肉类中的磺胺类药物进行色谱分离。我们实验室已经使用的两种分析方法在萃取和净化步骤以及液相色谱仪器方面未作任何改变的情况下进行了改进。在传统5 µm柱上应用的色谱条件已在填充2.6 µm核壳颗粒的柱上进行了优化。采用二元流动相[pH 4.50的醋酸盐缓冲溶液和甲醇 - 乙腈体积比为50:50的混合物],以梯度模式运行,流速为1.2 mL,进样体积为6 µL。这些色谱条件可在13分钟内完成13种磺胺类药物的分离。已经进行了初步研究,比较了饲料和肉类的空白样品和加标样品。两种基质的色谱图均实现了良好的分离度且无干扰。由于样品制备未作改变,优化后的方法无需进行全面重新验证,可用于加快常规分析速度。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/60b4/5225825/138bef1cc0d4/ijfs-2016-4-6166-g001.jpg

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