超高效液相色谱串联质谱法测定海参中硝基呋喃类代谢物残留量

Determination of Nitrofuran Metabolites in Sea Cucumber by Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry

目的:建立一种快速、准确、高效的超高效液相色谱串联质谱检测海参中硝基呋喃类代谢物残留量的方法。方法:采用40℃水浴中超声1 h,45℃气浴中衍生5 h,pH值7.0~7.5条件进行样品前处理,以2 mmol·L^(-1)乙酸铵的0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,超高效液相色谱串联质谱测定。结果:4种硝基呋喃类代谢物在0.5~20.0 ng·mL^(-1)线性关系良好,加标平均回收率在97.3%~103.6%,方法检出限为0.5μg·kg^(-1),定量限为1.0μg·kg^(-1)。结论:该方法可用于市售海参中硝基呋喃类代谢物残留量的快速检测。

Objective:To establish a rapid,accurate,and efficient method for detecting residual nitrofuran metabolites in sea cucumber using ultra-high performance liquid chromatography tandem mass spectrometry.Method:Sample pretreatment was carried out using ultrasound for 1 hour in a 40℃water bath,derivatization for 5 hours in a 45℃gas bath,and pH values ranging from 7.0 to 7.5.Gradient elution was performed using a mobile phase of 2 mmol·L^(-1)ammonium acetate in 0.1%formic acid aqueous solution acetonitrile,and ultra-high performance liquid chromatography tandem mass spectrometry was used for determination.Result:The four nitrofuran metabolites showed a good linear relationship in the range of 0.5 ng·mL^(-1)to 20.0 ng·mL^(-1),with an average recovery rate of 97.3%to 103.6%.The detection limit of the method was 0.5μg·kg^(-1),and the quantification limit was 1.0μg·kg^(-1).Conclusion:This method can be used for rapid detection of residual nitrofuran metabolites in commercially available sea cucumbers.