同位素内标法对水产品中硝基呋喃代谢物液相色谱-串联质谱法测定

Isotopic Internal Standard Method Determination of Nitrofuran Metabolics in Aquatic Products by Liquid Chromatograph-Tandem Mass Spectrometry

建立了水产品中硝基呋喃类代谢物残留量的同位素内标定量液相色谱-串联质谱法测定。样品经稀盐酸水解,邻硝基苯甲醛衍生,乙酸乙酯提取净化后,用液相色谱-串联质谱法通过正离子扫描多反应监测模式检测,稳定同位素内标定量。本方法的线性范围为1.25～10μg/kg,4种硝基呋喃代谢物的线性相关系数均在0.993 2以上,4种化合物的检测限为0.5μg/kg。在2.5 ng/mL、5 ng/mL、10 ng/mL 3个浓度水平加标平均回收率为81.6%～94.5%,RSD为5.4%～6.7%。结论证明该方法快速,灵敏度高,准确度、精密度好,满足样品测定的定性、定量要求。

An isotopic internal standard method determination of nitrofuran metabolics in aquatic products by liquid chromatograph-tandem mass spectrometry was developed.The sample was hydrolyzed by hydrochloric acid and the hydrolysate was derived from 2-Nitrobenzaldehyde.Then analytes was extracted by ethyl acetate and was detected with liquid chromatograph-tandem mass spectrometry in positive electro-sptray ionization using multiple reaction monitoring mode.The method used stable isotope internal standard quantitation.The scope of linear relationships was 1.25~10 μg/kg and correlation coefficients had all gone beyond 0.993 2.The limits of detection for four nitrofuran metabolics were 0.5 μg/kg.The average recoveries were 81.6%~94.5% and the related standard deviations were5.4%~6.7%at the three levels of 2.5 ng/mL、5 ng/mL、10 ng/mL.The results showed that this method was rapid,high sensitive,accurate and precise and can meet qualitative analysis with quantitative analysis.