摘要
建立了超声辅助衍生结合液相色谱/串联质谱（UAD-LC-MS/MS）快速测定水产养殖水体中4种硝基呋喃代谢物的方法。实验对比了超声辅助衍生和传统振荡衍生的效果,优化了色谱质谱条件以及衍生时间。水样经超声辅助的方式衍生,以2-硝基苯甲醛为衍生化试剂,再经乙酸乙酯提取,在正离子模式下以电喷雾电离串联质谱进行测定,内标法定量。在优化的实验条件下,4种代谢物在0.5～50 ng/m L范围内线性良好,相关系数〉0.998,方法检出限为0.02 ng/m L,定量限为0.05 ng/m L。在0.1,0.5和5 ng/m L的添加水平下,4种代谢物的平均回收率处于91.9%～104%之间,相对标准偏差（RSDs）处于2.1%～8.1%之间。测定了12份养殖水体中4种硝基呋喃代谢物的残留量,其中2份样本中检出呋喃西林代谢物氨基脲。方法可以准确测定养殖水体中硝基呋喃代谢物的残留量。
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. LC-MS / MS conditions,style and time of derivatization were conducted as improvements for the method. The samples were derivatized with 2-nitrobenzaldehyde by ultrasonic method,extracted with ethyl acetate,separated on a C18 column,confirmed by multiple reaction monitoring（ MRM） mode with electrospray ionization source using internal standard method. Under the optimized extraction conditions,the satisfactory recoveries for the blank water samples at three spiked levels（ 0. 1,0. 5 and 5 ng / m L） ranged from 91. 9% to104%,with the relative standard deviations of 2. 1% ~ 8. 1%. The limits of detection（ LODs） for the derivatized nitrofuran metabolites were 0. 02 ng / m L and the limits of quantification（ LOQs） were 0. 05 ng / m L.Good linearities were obtained over the range of 0. 5 ~ 50 ng / m L and the correlation coefficients（ R2） were better than 0. 998 for all compounds. The method was finally applied to detection of analytes in 12 real water samples,and semicarbazide（ SEM） that is metabolite of nitrofural was detected in two samples. The method is proved to be fast and effective for simultaneously qualitative and quantitative inspection of the metabolites of nitrofuran in fisheries water.
出处
《分析试验室》
CAS
CSCD
北大核心
2015年第4期416-420,共5页
Chinese Journal of Analysis Laboratory
基金
国家水产品质量安全风险评估项目(GJFP2014009)资助
