出口养殖水产品恶喹酸残留的HPLC监控、验证检测

The HPLC monitoring and confirmation of oxolinic acid residue in breeding fishes for export

本文介绍应用反相高效液相色谱(RP—HPLC)方法,对出口养殖水产品(活鳗鱼、大黄鱼、鲷鱼、鲈鱼)及烤鳗成品(包括烤串块、肚串)的恶喹酸残留进行的大量连续监控、验证检测。试验结果表明,在相同的分离纯化试验条件下,烤鳗与活鳗之间、不同水产品品种之间HPLC图谱特点显示样品弱保留成分不同,对结果定性的干扰程度不同,可采用不同色谱条件实现充分的分离。经实验筛选,在流动相40％乙腈+60％25mmolNaH_2PO_4,pH3.0,流速0.8mL/min的色谱条件下鲜活样品干扰成分较易分离,恶喹酸保留时间适中,单样上机分析周期8分钟,适用于大量快速监控检测;而在30％乙腈+70％25mmol NaH_2PO_4,pH3.0,流速0.8mL/min的色谱条件下恶喹酸保留时间相对较长,单样分析周期15分钟,适合于大多数供试样品的恶喹酸验证和定量。该方法的添加浓度为50μg/kg时,回收率70％～95％。分析讨论了恶喹酸快速监控中的定性分析问题。

In this article, with the RP-HPLC method a mass and serial monitoring and confirmation were taken to study the oxolinic acid residues in breeding fishes and processing product for export (including eels, yellow croaker and other fishes etc.).The result shows that with the same separation and purification the chromatograph characteristic differs in between roasting eel and live eel or among the different fishes.Due to the different weak retention component the disturbing peak differs.Therefore under the different chromatography condition, the satisfying separation can be achieved.In detail with the condition in live fishes sample: mobile phase 40% acetonitrile+60% 25mmol sodium dihydrogen phosphate pH 3.0, flow rate 0.8mL/min, the disturbing factor can be easily eliminated and the retention time of oxolinic acid is medial.It takes eight minutes to analyze a single sample, which is suitable to a mass of quick analysis for monitoring.While with the conditon that mobile phase 30%acetonitrile+70% 25mmol sodium dihydrogen phosphate, pH3.0, flow rate 0.8mL/min the single sample analysis costs fifteen minutes, which is suitable to the qualitative and quantitative analysis for the most samples.With the fortified level of 50μg/kg, the recoveries for this method ranges from 70% to 95%.Besides the confirmative method also is discussed in this article.