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微波辅助提取和原位净化-液相色谱串联质谱法测定鸡肉中氟喹诺酮类抗生素。

Microwave-assisted extraction and in situ clean-up for the determination of fluoroquinolone antibiotics in chicken breast muscle by LC-MS/MS.

机构信息

College of Chemistry, Jilin University, Changchun, P. R. China.

出版信息

J Sep Sci. 2011 Jan;34(2):142-9. doi: 10.1002/jssc.201000365. Epub 2010 Dec 7.

DOI:10.1002/jssc.201000365
PMID:21246719
Abstract

A new method was developed for the determination of six fluoroquinolone antibiotics including fleroxacin, levofloxacin, ciprofloxacin, lomfloxacin, enrofloxacin, and sparfloxacin in chicken breast muscle, in which the extraction and clean-up were performed in one step by microwave irradiation. The mixture of ACN containing 0.3% v/v phosphoric acid/water pH 3 (70:30, v/v) was used as the extraction solution and hexane was used as the clean-up solution. The extract was analyzed by liquid chromatography-tandem mass spectrometry system. The RSDs of intra- and inter-day obtained are in the range of 1.0-10.4 and 3.8-13.6%, respectively. In the three fortified levels of chicken breast muscle (20, 100, and 500 ng/g), the recoveries of fluoroquinolone antibiotics ranging from 66.0 to 97.2% are obtained. The LODs are in the range of 2.7-6.7 ng/g. This method simplifies the process of the sample preparation and reduces the operation errors.

摘要

建立了一种新的方法,用于测定鸡肉中 6 种氟喹诺酮类抗生素,包括氟罗沙星、左氧氟沙星、环丙沙星、洛美沙星、恩诺沙星和司帕沙星。该方法采用微波辐射,一步提取和净化。提取液为含 0.3%(v/v)磷酸的乙腈/水(pH 3,70:30,v/v)溶液,正己烷作为净化液。采用液相色谱-串联质谱系统进行分析。该方法的日内和日间精密度的 RSD 分别在 1.0-10.4%和 3.8-13.6%范围内。在鸡肉中 3 个加标水平(20、100 和 500ng/g)下,氟喹诺酮类抗生素的回收率在 66.0-97.2%之间。检出限在 2.7-6.7ng/g 之间。该方法简化了样品前处理过程,减少了操作误差。

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