高效液相色谱法检测鸡肉中四种氟喹诺酮类药物残留的研究

Determination of four fluoroquinolones drugs in Chicken by High performance Liquid Chromatography

关键词:  鸡肉  氟喹诺酮类药物  高效液相色谱法

Key words:  Chicken  fluoroquinolones drugs  High performance Liquid Chromatography

摘要:

本试验旨在建立一种反相液相色谱法同时测定鸡肉中四种氟喹诺酮类药物残留的分析方法。禽肉肉样在PH中性条件下用乙腈提取，正己烷去杂质，蒸发浓缩后，流动相定容，用激发波长是280 nm，发射波长是450 nm的荧光检测器测定。氧氟沙星(Ofloxacin),在0.003 ug/g-0.6 ug/g范围内呈良好的线性关系，诺氟沙星(Norfloxacin)、环丙沙星(Ciprofloxacin)、恩诺沙星(Enrofloxacin)在 0.001 ug/g-0.2 ug/g范围内呈良好的线性关系，检出限分别为：氧氟沙星 0.006 μg/ml，诺氟沙星、环丙沙星、恩诺沙星0.002 μg/ml。定量限分别为：氧氟沙星 0.015 μg/ml，诺氟沙星、环丙沙星、恩诺沙星0.005 μg/ml。添加0.006 ug/g-1.50 ug/g浓度水平，氧氟沙星平均添加回收率范围为59 %~95 % ；添加0.002 ug/g-0.5 ug/g浓度水平，诺氟沙星、环丙沙星、恩诺沙星平均添加回收率范围分别为57 %~95%，56 %~92 %，70 %~105 % 。相对标准偏差在 15 %以内。 此建立的方法操作简单，分离效果好，检出限低，重现性好，能成功用于测定禽肉中的喹诺酮类药物残留。

Abstract:

A reversed-phase HPLC method was developed for the quantitative analysis of fluoroquinolones drugs in poultry meat. Samples were extracted with acetonitrile in PH7.0. The sample extracts were cleaned up by Hexane, then enriched by evaporation and determined by fluorescence detection at 280nm (EX) and 450nm (EM). Over the concentration range 0.003ug/g-0.6ug/g of Ofloxacin(OFLX), 0.001ug/g-0.2ug/g of Norfloxacin(NOR)、Ciprofloxacin(CIF)、Enrofloxacin(ENR), the calibration curves were liner. Limit of detection was 6ng/g For OFLX, 2ng/g for NOR、CIF 、ENR. Quantity limit of detection was 15ng/g For OFLX, 5ng/g for NOR、CIF 、ENR. Average recoveries at three fortification levels in the range 0.006ug/g-1.50ug/g or 0.002ug/g-0.5ug/g in poultry meat , The average recovery was the range of 59%~95% for OFLX, 57%~95% for NOR, 56%~92% for CIF, 70%~105% for ENR . Coefficients of variation was 15% . The method is simple, better degree of separation, low limit of drugs in poultry meat successfully.