国家标准方法测定水产品中硝基呋喃类代谢物残留量检测方法的改进

Improvement of National Standard Method for Determination of Residual Nitrofuran Metabolites in Aquatic Products

针对水产品硝基呋喃类药物代谢物我国农业农村部制定了783-1-2006号公告,使用液相色谱串联质谱法检测水产品中硝基呋喃类代谢物。该方法是将样品肌肉组织残留的硝基呋喃类代谢物在酸性条件下水解衍生化,经液液萃取后,内标法定量。本方法前处理简单,液液萃取避免了固相萃取的繁琐,减少了目标化合物的损失,内标法校正使得结果较为准确。但是,仍存在衍生化过程酸度不够导致衍生化不够彻底,提取过程磷酸氢二钾浓度不够导致提取不彻底,甲醇溶液定容后,涡旋振荡溶解出现乳化现象等问题。结合实际情况对国家标准方法进行改进和优化,进一步提升方法的准确度、精密度、灵敏度。

The ministry of agriculture of China has formulated bulletin 783-1-2006 to detect the nitrofuran metabolites of aquatic products by liquid chromatography series mass spectrometry.The method is to hydrolyze the nitrofuran metabolites remaining in the muscle tissue of the sample under acidic conditions.After liquid extraction,the internal standard method quantifies it.The pretreatment is simple,liquid extraction avoids the complexity of solid phase extraction,reduces the loss of target compounds,and the internal calibration method makes the results more accurate.However,there are still problems such as insufficient acidity in the derivative process leading to incomplete derivation,insufficient concentration of potassium dihydrogen phosphate in the extraction process leading to incomplete extraction,and finally,after the methanol solution is fixed,emulsifying phenomenon occurs in vortex oscillation dissolution.The national standard method is improved and optimized according to the actual situation.The accuracy,precision and sensitivity of the method were further improved.