摘要
采用超高压液相色谱-三重串联四级杆质谱仪优化了渔业养殖水和底泥中4种硝基呋喃代谢物残留检测的方法。确定以2-硝基苯甲醛为衍生剂,样品经60℃高温振荡衍生4 h,再经乙酸乙酯提取,C_（18）色谱柱分离,在正离子反应模式下以大气压电喷雾源电离,采用多反应监测,内标法定量。方法中4种硝基呋喃代谢物的检出限为0.1 ng/mL（g）,定量限为0.25 ng/mL（g）,在0.25~10 ng/mL（g）线性范围良好,0.5、2.0、5.0 ng/mL（g）3个添加水平回收率范围为91.3%~102.2%,相对标准偏差均小于10%。本方法具有重复性好、灵敏度高、简便、准确以及快速的优点,可以满足渔业养殖环境中硝基呋喃类药物残留的监控要求。
A rapid method based on ultrasound assisted derivatization（ UAD） with high performance liquid chromatography- tandem mass spectrometry was proposed for determination of 4 nitrofuran metabolite residues in fisheries water and sediment. It was determined that 2- nitrobenzaldehyde was used as a derivating agent. The sample was derived after 60 ℃ oscillation for 4 h. It was then extracted by ethylacetate and separated by a C18 column. It was confirmed by multiple reaction monitoring（ MRM） mode with electrospray ionization source using internal standard method. Under the optimized extraction conditions,the limits of detection（ LODs） for the derivatized nitrofuran metabolites were 0. 1 ng / m L and the limits of quantification（ LOQs） were 0. 25 ng / m L（ g）. Good linearities were obtained over the range of 0. 25 - 10 ng / m L（ g）. The satisfactory recoveries for the blank water samples at three spiked levels（ 0. 5,2. 0 and 5. 0 ng / m L（ g）） ranged from 91. 3% to 102. 2%,with all relative standard deviations under 10%. The method is proved to be fast and effective for simultaneously qualitative and quantitative inspection of the metabolites of nitrofuran in fisheries environment.
出处
《中国渔业质量与标准》
2016年第4期37-43,共7页
Chinese Fishery Quality and Standards
基金
扬州市绿扬金凤计划资助(扬人才办[2014]5号)
关键词
硝基呋喃代谢物
液质联用
养殖环境
底泥
衍生温度
nitrofuran metabolites
derivatization temperature
fisheries environment
sediment
UPLC-MS / MS
