超高效液相色谱-质谱内标法同时测定海洋药用生物中硝基呋喃类代谢物残留量

Simultaneous determination of four nitrofuran metabolites in marine drug organisms by UPLC MS/MS method with internal standard

目的:建立测定海洋药用生物中4种硝基呋喃类药物(呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因)代谢物的超高效液相色谱-串联质谱方法。方法:硝基呋喃类代谢物经过二硝基苯甲醛衍生化,用乙酸乙酯提取,经液相色谱分离,串联四极杆质谱多反应监测(MRM)模式检测,内标法定量。结果:4种硝基呋喃类代谢物线性范围为0.5～20.0μg.L-1,相关系数均大于0.99,定量限在0.06～0.37μg.kg-1范围内,加标回收率为90.2%～101.6%,RSD为2.9%～4.8%。结论:该方法前处理简单,灵敏度和准确度高,适合对海洋药用生物中硝基呋喃类代谢物残留的检测。

Objective： To develop a UPLC-MS /MS method for the simultaneous determination of four nitrofuran metabolites（furazolidone,furaltadone,nitrofurazone and nitrofurantoin） in marine drug organisms.Methods： Samples were derivatized with 2-nitrobenzaldehyde and extracted by ethyl acetate.The analytes were separated using UPLC and detected by multi-reactions monitoring（MRM） technology of tandem mass spectrometry with electrospray ionization source.Results： The calibration curve of four nitrofuran metabolites showed good linearity in the range of 0.5 20.0 μg.L-1,and correlation coefficient were all above 0.99.The limits of quantification for four nitrofuran metabolites in samples were between 0.06 and 0.37 μg.kg-1.The average recoveries at three levels（0.5、1.0、5.0 μg.kg-1） ranged from 90.2 %-101.6 % with RSD 2.9 % to 4.8 %.Conclusion： The established method is simple,sensitive and accurate,which is suitable for the determination of four nitrofuran metabolites in marine drug organisms.