超声波辅助衍生-液相色谱串联质谱法快速测定克氏原鳌虾中的硝基呋喃类代谢物残留

Rapid Determination of Nitrofuran Metabolites in Procambarus clarkii by Ultrasonic Assisted Derivatization-liquid Chromatography Tandem Mass Spectrometry

建立了克氏原鳌虾样品中4种硝基呋喃类代谢物残留检测的超声波辅助衍生-液相色谱串联质谱法。试验对比了超声波辅助衍生和恒温振荡衍生的效果,优化了色谱质谱条件以及定性定量离子对,确定了最佳试验条件。在优化的实验条件下,4种硝基呋喃类代谢物在0.5~50.0 ng/mL范围内线性良好,相关系数>0.99,方法检出限为0.5μg/kg,在3个不同质量浓度的添加水平下,4种代谢物的平均回收率在93.3%~104.9%之间,相对标准偏差<10%。采用实际样品对本文所建立的方法和国家标准检验方法对比,结果表明两种方法所测得的样品含量偏差较小,小于4.78%,本方法相较于国标方法更为简便快速,能显著缩短样品前处理时间,提高检测效率,在日常检测方面存在一定的优势,可为后续开展进一步的基础研究奠定基础。

An ultrasonic-assisted derivatization-liquid chromatography-tandem mass spectrometry method for rapid determination of four nitrofuran metabolites in Procambarus clarkii was established. The derivatization effects of ultrasonic assisted and constant temperature oscillation were compared. The conditions of chromatography-mass spectrometry and qualitative and quantitative ion pairs were optimized, and the best experimental conditions were determined. Under the optimized experimental conditions, 0.5~50.0 ng/mL was the linear range of the four metabolites, the correlation coefficient was greater than 0.99, and the detection limit of the method was 0.5 μg/kg. The average recoveries of the four metabolites ranged from 93.3% to 104.9% and the relative standard deviation was less than 10%. The results show that the deviation of the two methods is less than 4.78%. Compared with the national standard method, this method is more simple and rapid, which can significantly shorten the sample pretreatment time and improve the detection efficiency. It has some advantages in daily detection, and can provide a basis for further development and lay the foundation for basic research.