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高效液相色谱(HPLC)串联质谱法快速测定鱼和猪肌肉中 19 种喹诺酮类残留。

Rapid determination of 19 quinolone residues in spiked fish and pig muscle by high-performance liquid chromatography (HPLC) tandem mass spectrometry.

机构信息

School of Food Science and Technology, Southern Yangtze University, Wuxi, China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Mar;26(3):306-13. doi: 10.1080/02652030802484851.

Abstract

A multiresidue method has been developed for the confirmation and quantification of 19 quinolones (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, flumequine, oxolinic acid, difloxacin, sarafloxacin, sparfloxacin, danofloxacin, fleroxacin, marbofloxacin, enoxacin, orbifloxacin, pefloxacin, nalidixic acid, pipemidic acid, lomefloxacin and cinoacin) in pig and fish by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile, analytes separated by LC on a C18 column using 0.1% formic acid-methanol with a linear gradient elution programme, and detected by MS/MS. The linear range was 0.3-50 microg kg(-1) with correlation coefficients (r) more than 0.9956. The limits of detection were 0.1 microg kg(-1). Mean recoveries for each analyte in pig muscle and fish ranged from 75.3% to 96.3% and from 79.7% to 94.2% with relative standard deviations below 10%. The method is fast, safe, sensitive and precise, and can be used simultaneously to analyse residual quinolones.

摘要

已建立了一种多残留方法,用于通过液相色谱-串联质谱法(LC-MS/MS)确认和定量检测猪和鱼中的 19 种喹诺酮类药物(恩诺沙星、环丙沙星、诺氟沙星、氧氟沙星、氟甲喹、恶喹酸、双氟沙星、沙拉沙星、司帕沙星、丹诺沙星、二氟沙星、马波沙星、恩诺沙星、奥比沙星、培氟沙星、萘啶酸、吡哌酸、洛美沙星和 cinoxacin)。样品用乙腈提取,用 C18 柱通过 LC 分离,使用 0.1%甲酸-甲醇进行线性梯度洗脱程序,并用 MS/MS 检测。线性范围为 0.3-50 μg kg(-1),相关系数(r)大于 0.9956。检测限为 0.1 μg kg(-1)。猪肌肉和鱼中每种分析物的平均回收率在 75.3%至 96.3%之间,相对标准偏差低于 10%。该方法快速、安全、灵敏、准确,可同时用于分析残留的喹诺酮类药物。

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