液相色谱串联质谱法测定巴鱼中硝基呋喃代谢物的残留量

Determination of nitrofuran metabolic residues in Spanish mackerel by liquid chromatographytandem mass spetrometry

建立巴鱼中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因的代谢物残留量液相色谱-串联质谱的方法。分析物采用电喷雾电离正离子（ ESI ＋）、多反应监测（M RM ）模式检测，内标法定量。本实验对固相萃取法提取和乙酸乙酯提取净化前处理方法进行比对，4种硝基呋喃代谢物的混合标准溶液的浓度在0.5～50ng/mL范围线性良好，相关系数均大于0.9981，4种化合物的检测限为0.5μg/kg。添加浓度1μg/kg、2.5μg/kg、5μg/kg范围内得出4种代谢物固相萃取净化法的回收率在81.1％～104.1％之间，相对标准偏差（RSD）小于5.7％.乙酸乙酯提取净化法的回收率在88.5％～108.2％之间，相对标准偏差（RSD ）小于6.1％。结论证明乙酸乙酯提取法方法前处理简单、快速、稳定性好，适用于大量样品的同时检测。

A method was established to detect nitrofuran metabolic residues in Spanish mackerel by liq-uid chromatography tandem mass spetrometry （LC-MS/MS） .Theanalvtes were detected by LC-MS/MS （ESI） with multiple reaction monitoring （MRM ）.The result indicated that the calibration curves were in good linearity between the peak area and the concentration of 0.5-50ng/ml for nitrofuran metabolic with correlation cofficients not less than 0.9981.The limits of detection for four nitrofuran metabolics were 0.5μg/kg. .Then analytes were extracted by spe or ethyl acetat the average recoveries were 81.1%-104.1% or 88.5%-108.2% and the related standard deviations less than 5.1 or 6.1% at the three levels 1μg/kg、2.5μg/kg、5μg/kg.The proposed method was simple ,rapid ,the stability was good and suitable for the simultaneous quantitative detection.