酶联免疫法与LC-MS/MS法测定水产品中呋喃唑酮代谢物

Enzyme Linked Immunosorbent Assay(ELISA) and LC-MS/MS for Determination of Furazolidone Residues in Aquatic Products

运用酶联免疫法和LC-MS/MS法对水产品中呋喃唑酮代谢物残留进行测定。样品经2-硝基苯甲醛衍生化并用乙酸乙酯提取。向样品中分别添加0.60、2.00、6.00μg/kg三个浓度水平的呋喃唑酮代谢物时,酶联免疫法平均回收率分别为99.2%、96.0%和100.0%,变异系数(RSD)为1.8%～12.6%,最低检测限为0.3μg/kg。LC-MS/MS法平均回收率分别为90.8%、94.3%和86.3%,RSD为6.2%～14.3%,最低检测限为0.1μg/kg。用酶联免疫法对150个样品进行检测,筛选出3个阳性样品,经LC-MS/MS确证为阳性,未发现假阳性样品,且测定结果基本一致。研究表明酶联免疫法重复性较好、准确度较高,是一种水产品中呋喃唑酮代谢物残留的快速筛选方法;液-质/质联用法灵敏度高,适用于阳性样品的确证和精确定量。

ELISA and LC-MS/MS for the analysis of furazolidone （AOZ） residues in aquatic products were studied. Samples were derivatived with 2-nitrobenzaldehyde and extracted with ethyl acetate. When the samples were spiked with 0.60, 2.00 and 6.00 μg/kg of AOZ, the average recoveries are 99.2%, 96.0% and 100.0% respectively by ELISA, while the relative standard deviation（RSD） is 1.8%～12.6% with detection limit of 0.3μg/kg. The average recoveries are 90.8%, 94.3% and 86.3% respectively by LC-MS/MS and RSD is 6.2%～ 14.3% with detection limit of 0.1 μ g/kg. Three positive samples analyzed by ELISA were confirmed by LC-MS/MS and no false positive samples were found. The results are basically the same. The results showed that ELISA is a rapid and exact method with good reproducibility suitable for the screen of AOZ positive samples in aquatic products. Hence LC-MS/MS is sensitive and suitable for determination of positive samples.