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高效液相色谱-集成脉冲安培检测法测定原料乳中的头孢匹林和氨苄青霉素

Assay for cephapirin and ampicillin in raw milk by high-performance liquid chromatography--integrated pulsed amperometric detection.

作者信息

Dasenbrock C O, LaCourse W R

机构信息

Department of Chemistry and Biochemistry, University of Maryland, Baltimore 21250, USA.

出版信息

Anal Chem. 1998 Jun 1;70(11):2415-20. doi: 10.1021/ac971375e.

DOI:10.1021/ac971375e
PMID:9624911
Abstract

The FDA has issued guidelines governing the use of antibiotics in cattle and routinely tests for the presence of antibiotics in milk. Unfortunately, these compounds are often difficult to detect by direct methods because they often lack a chromophore or fluorophore. Integrated pulsed amperometric detection (IPAD) following reversed-phase liquid chromatography is well-suited for this analysis because it is selective, sensitive, and direct; i.e., derivatization is not required. This work involves the development of a simple, rapid assay for the determination of beta-lactam antibiotic residues in milk using HPLC-IPAD, specifically, ampicillin and cephapirin. Since the analyst studied here are detectable by UV detection, a comparison between IPAD and UV detection will be made. Sample preparation schemes that involve the extraction of antibiotics of interest from the milk matrix and subsequent cleanup are an important aspect of this project. These procedures will be discussed in detail. In addition, analytical figures of merit and IPAD wave form optimization will be addressed.

摘要

美国食品药品监督管理局(FDA)已发布关于牛用抗生素使用的指导方针,并定期检测牛奶中抗生素的存在情况。不幸的是,这些化合物通常难以通过直接方法检测,因为它们往往缺乏发色团或荧光团。反相液相色谱后的积分脉冲安培检测(IPAD)非常适合这种分析,因为它具有选择性、灵敏且直接;即无需衍生化。这项工作涉及开发一种简单、快速的测定牛奶中β-内酰胺类抗生素残留的方法,使用高效液相色谱-积分脉冲安培检测(HPLC-IPAD),具体为氨苄青霉素和头孢匹林。由于此处研究的分析物可通过紫外检测进行检测,因此将对积分脉冲安培检测(IPAD)和紫外检测进行比较。从牛奶基质中提取目标抗生素并随后进行净化的样品制备方案是该项目的一个重要方面。将详细讨论这些程序。此外,还将讨论分析性能指标和积分脉冲安培检测(IPAD)波形优化。

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