首页> 中文期刊>淡水渔业 >淡水养殖用水中硝基呋喃代谢物残留量的 UPLC/MS/MS 检测方法

淡水养殖用水中硝基呋喃代谢物残留量的 UPLC/MS/MS 检测方法

     

摘要

An ultra performance liquid chromatography-tandem mass spectrometric ( UPLC/MS/MS) method was established for determining 4 nitrofuran metabolites in freshwater, namely 1-aminohydantoin hydrochloride (AHD) , 3-amino-5-morpholinomethyl-2-oxazolidineone (AMOZ), 3-amino-2-oxazolidinone (AOZ) and semicarbazide (SEM). The samples were subjected with dilute hydrochloric acid then derivatized with 2-nitrobenzene formaldehyde. The analysis was carried out in the multi reaction monitoring ( MRM) mode and internal standard isotope dilution method was used for quantification. Calibration curves exhibited good linearity over the concentration range from 1. 0 to 100 ng/mL and their limits of detection were all 0. 5 μg/L. Average recoveries for them spiked at 4 levels ranged from 75. 1% to 102% , with a RSD of less than 15%.%研究了淡水养殖用水中4种硝基呋喃代谢物:呋喃唑酮代谢物(AOZ)、呋喃它酮代谢物(AMOZ)、呋喃妥因代谢物(AHD)、呋喃西林代谢物(SEM)的超高效液相色谱-串联质谱(UPLC/MS/MS)分析方法.以邻硝基苯甲醛作为衍生化试剂,D4-AOZ、D5-AMOZ、13C15N-SEM、13C-AHD作内标,用水解衍生的方法对样品进行处理.以乙腈和0.1%甲酸(含有0.5mmol/mL乙酸铵)水溶液为流动相,采用梯度洗脱,4.5min可将4种代谢物完全分离,进行定性和定量分析.加标回收率为75.1%~102%;本方法的检出限(LOD)为0.50μg/L.

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