超高效液相色谱-串联质谱法检测中华圆田螺硝基呋喃代谢物残留量

Determination of nitrofuran metabolites residues in Cipangopaludina cahayensis by ultra high performance liquid chromatography-tandem mass spectrometry

目的建立了超高效液相色谱-串联质谱法同时测定中华圆田螺中呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林4种硝基呋喃代谢物的方法。方法样品经50%甲醇水洗涤除杂后,进行衍生,用磷酸氢二钾溶液调pH后,经过乙酸乙酯提取,氮吹浓缩,乙酸铵和乙腈混合溶液定容,且正己烷除脂,吸取下层液体过膜待测。在正离子模式下,采用多反应监测模式同时测定中华圆田螺中的4种硝基呋喃代谢物。结果在优化后的仪器工作条件下进行测定,4种代谢物的质量浓度在1.0~10 ng/mL的范围内线性关系良好,相关系数为0.9994~0.9998,检出限为1.07×10^-2~7.02×10^-2 ng/g。加标回收率为92.0%~104.0%,批内和批间相对标准偏差均小于10%,测定结果的相对标准偏差为0.7%~4.7%(n=6)。结论该方法具有良好的精密度、准确度和重现性,可用于同时测定中华圆田螺中的呋喃唑酮、呋喃它酮、呋喃妥因和呋喃西林4种硝基呋喃代谢物。

Objective To establish a method for simultaneous determination of the four metabolites of furazolidone,furaltadone,furantoin and furacilin in Cipangopaludina cahayensis by ultra high performance liquid chromatography–tandem mass spectrometry(UPLC–MS/MS).Methods The sample was washed and purified with 50%methanol water,and then derived.After pH was adjusted with dipotassium hydrogen phosphate solution,the sample was extracted by ethyl acetate,concentrated by nitrogen blowing,mixed with ammonium acetate and acetonitrile at a constant volume,and hexane was lipid removed.The lower liquid was absorbed through the membrane to be measured,and four nitrofuran metabolites in Cipangopaludina cahayensis were determined simultaneously in the positive ion mode by the multi-reaction monitoring mode.Results Under optimized instrument operating conditions,four kinds of nitrofuran metabolites had good linear relationship in the range of 1.0-10 ng/mL,the correlation coefficients were 0.9994-0.9998,the limits of detection were 1.07×10^-2-7.02×10^-2 ng/g.The average recovery rates were 92.0%-104.0%.Relative standard deviations within and between batches were less than 10%,and the relative standard deviations of determination results were 0.7%-4.7%(n=6).Conclusion The method has good precision,accuracy,and reproducibility,and it is suitable for thedetermination of four metabolites of furazolidone,furaltadone,furantoin and furacilin in Cipangopaludina cahayensis at the same time.