液相色谱串联质谱法检测水产品硝基呋喃类代谢物的改进

国标GB/T 20752—2006测定水产品硝基呋喃类药物代谢物的实际回收率为40%左右、线性范围0.2～2μg/kg。为改进不足，本实验改用乙酸乙酯提取、液液萃取净化，并适当改变LC-MS/MS检测中液相色谱条件和质谱条件，结果显示，样品前处理时间大大缩短，方法回收率81.3%～106.0%，相对标准偏差小于11%，线性范围0.1～4.0μg/kg，相关系数0.999以上，最低检出限0.1μg/kg。改进后的方法比国标方法在准确度、灵敏度和稳定性等方面均有所提高。

Improved Liquid Chromatography-Tandem Mass Spectrometric Method for Determination of Nitrofuran Metabolites Residues in Aquatic Products

The Chinese national standard method, GB/T 20752—2006 has been used for the determination of nitrofuran metabolites residues in aquatic products using liquid chromatography-tandem mass spectrometry (LC-MS/MS), with a recovery rate of 40% and a linear range of 0.2－2 μg/kg. Extraction of test portions with ethyl acetate followed by clean-up using liquid-liquid extraction was adopted and appropriate adjustments of LC-MS/MS conditions were conducted as improvements for the method. Results showed that the pretreatment time was shortened, and the average spike recovery rates for six replicate determinations were elevated to 81.3%－106.0%, with a RSD of less than 11%. This method exhibited a linear range of 0.1－4 μg/kg (r2 > 0.999) and a limit of detection of 0.1 μg/kg.