快速滤过型净化法结合超高效液相色谱串联质谱法测定动物源性食品中四唑虫酰胺残留

Determination of tetraniliprole residues in animal derived foods by multi-plug filtration cleanup combined with HPLC-MS/MS

[目的]建立一种准确、快速测定动物源性食品中四唑虫酰胺残留量的分析方法。[方法]样品经乙腈提取,氯化钠和无水硫酸镁盐析分层,上层经m-PFC净化,高效液相色谱质谱联用仪测定,外标法定量。[结果]四唑虫酰胺在0.001~0.150 mg/L范围内线性良好,相关系数均>0.999,定量限为0.002 mg/kg;以猪肉、牛肉、羊肉、鸡肉、猪肝、牛肝、羊肝、鸡肝、鸡蛋、牛奶阴性样品为基质,四唑虫酰胺的平均加标回收率为90.0%~108.0%,相对标准偏差为1.10%~4.89%。[结论]该方法适用于动物源性食品中四唑虫酰胺的定量分析。

[Objective]This study aimed to develop a rapid and efficient method for quantifying tetraniliprole residues in animal-derived foods by combining multi-plug filtration cleanup(m-PFC)with high-performance liquid chromatography-mass spectrometry(HPLC-MS).[Methods]Samples were extracted with acetonitrile,followed by salting out using sodium chloride and anhydrous magnesium sulfate.The extracts were purified via m-PFC and analyzed using HPLC-MS with external standard calibration.[Results]The method demonstrated a strong linear correlation between tetraniliprole concentration and response values over a range of 0.001 to 0.150 mg/L,with a coefficient of determination(R2)exceeding 0.999.The limit of quantification(LOQ)was 0.002 mg/kg.Average recovery rates ranged from 90.0%to 108.0%,with relative standard deviations between 1.10%and 4.89%,validated across a variety of matrices,including pork,beef,mutton,chicken,pork liver,beef liver,mutton liver,chicken liver,eggs and milk.[Conclusion]The proposed method is rapid,straightforward,high sensitivity,and suitable for quantitative determination of tetraniliprole residues in animal-derived food.