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亲水作用色谱-离子对色谱法测定牛奶中链霉素和双氢链霉素残留量的研究。

Hydrophilic interaction vs ion pair liquid chromatography for the determination of streptomycin and dihydrostreptomycin residues in milk based on mass spectrometric detection.

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimiopolis Zografou, Athens, Greece.

出版信息

J Chromatogr A. 2010 Oct 22;1217(43):6646-51. doi: 10.1016/j.chroma.2010.04.059. Epub 2010 Apr 28.

Abstract

Streptomycin (STR) and dihydrostreptomycin (DHSTR) are two of the most common aminoglycoside antibiotics used in veterinary medicine. The physicochemical properties of both substances, make their determination challenging. In the present study the development of methods based on ion-pair chromatography (IPC) and on hydrophilic interaction chromatography (HILIC), for the determination of the above mentioned aminoglycosides in the range of 100-1000 μg L(-1) is described. The two methods were validated according to EU requirements for residues in food. The recoveries for the IPC method were 69.3% and 56.5% of STR and DHSTR, respectively, and for HILIC method 85.5% and 72.3%, respectively. The intra- and inter-day precision, studied at 100, 200 and 300 μg kg⁻¹ levels in milk samples, gave %RSD ≤ 13 for both methods. LOQs for the HILIC method were 14 μg kg⁻¹ for both analytes and for the IPC method were 109 and 31 μg kg⁻¹, for STR and DHSTR, respectively. The sensitivity of the HILIC method is 80 and 210 times greater than that of the ICP method, for STR and DHSTR, respectively.

摘要

链霉素(STR)和双氢链霉素(DHSTR)是兽医中最常用的两种氨基糖苷类抗生素。这两种物质的物理化学性质使得它们的测定具有挑战性。本研究描述了基于离子对色谱(IPC)和亲水相互作用色谱(HILIC)的方法的开发,用于在 100-1000μg L(-1)范围内测定上述氨基糖苷类抗生素。这两种方法均根据欧盟对食品中残留物的要求进行了验证。IPC 方法的回收率分别为 STR 和 DHSTR 的 69.3%和 56.5%,HILIC 方法的回收率分别为 85.5%和 72.3%。在牛奶样品中在 100、200 和 300μg kg(-1)水平下研究的日内和日间精密度,两种方法的%RSD≤13。HILIC 方法的 LOQ 对于两种分析物均为 14μg kg(-1),而 IPC 方法的 LOQ 分别为 STR 和 DHSTR 的 109 和 31μg kg(-1)。HILIC 方法的灵敏度分别比 ICP 方法高 80 和 210 倍,用于 STR 和 DHSTR。

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