超高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物残留

Determination of nitrofuran metabolite residues in aquatic products by ultra performance liquid chromaography-tandem mass spectrometry

采用超高效液相色谱-串联质谱法(UPLC-MS/MS)检测了水产品中硝基呋喃代谢物残留。样品经盐酸溶液水解和2-硝基苯甲醛衍生后,用乙酸乙酯萃取、浓缩后,以甲醇、水(20?80)溶液定容,经Acquity BEHC18超高压液相色谱柱分离,用电喷雾电离(ESI)串联四极杆质谱仪以多反应监测扫描模式(MRM)进行检测分析。实验中,对液-质分离条件和样品前处理条件进行了优化。结果表明,4种硝基呋喃代谢物在1.0～10μg/L浓度范围内呈良好线性关系(r≥0.9959),定量限范围为0.1～0.7μg/kg。该方法简便、快速、灵敏,测定结果能满足水产品硝基呋喃代谢物残留的检测要求。

Ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was applied to the simultaneous determination of nitrofuran metabolite residues in aquatic products.Samples were dissolved in hydrochloric acid solution and derivatized with 2-nitrobenzaldehyde.After extraction and inspissated with ethyl acetate,the analytes were dissolved with methanol solution（CH3OH ：H2O=20 ：80）.The separation was performed on an Acquity BEH C18 UPLC column under gradient elution and the detection was performed by an electrospray ionization tandem quadrupole mass spectrometer with multiple reaction mode.The separation and the sample pretreatment conditions were optimized.The results showed that there was a good linear relationship in the range of 1.0～10μg/L（r=0.9959）,and the limit of quantification was 0.1～0.7μg/L.The method is easy,rapid and sensitive.