QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中30种抗寄生虫类药物残留

Determination of 30 Kinds of Antiparasitic Drugs in Animal-derived Foods by QuEChERS-UPLC-MS/MS

目的:采用超高效液相色谱-串联质谱法,建立测定动物源性食品中30种抗寄生虫类药物残留的方法。方法:样品经乙腈、1%氨水乙酸乙酯提取,经QuEChERS净化。净化后采用Waters ACQUITY UPLC^(TM) BEH C_(18)色谱柱分离,10 mmol/L甲酸铵(含0.1%甲酸)水溶液-乙腈:甲醇(50:50,v:v)为流动相进行梯度洗脱,电喷雾离子源正负离子切换多反应监测(Multiple Reaction Monitoring,MRM)模式下进行检测,基质匹配外标法定量。结果:在优化的条件下,30种抗寄生虫类药物在各自的线性范围内线性良好,决定系数(r^(2))均大于0.99;回收率为70.1%~111%;相对标准偏差在0.10%~9.1%之间(n=6);方法检出限为0.001~0.3μg/kg之间,方法定量限在0.004~1μg/kg。结论:该方法灵敏、准确,具有良好的重复性和稳定性,可用于动物源性食品中多种抗寄生虫药物残留的检测。

Objective:A method for determining the residues of 30 antipa rasitic drugs in animal-derived food using ultrahigh-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Methods:The samples were extracted with acetonitrile and 1%ammonia acetic ether and purified by QuEChERS.After purification,Waters ACQUITY UPLC^(TM) BEH C_(18) column was used for separation,and a gradient elution of 10 mmol/L ammonium formate(containing 0.1%formic acid)aqueous solution,acetoni trile:methanol(50:50,v:v)was performed as the mobile phase.Detection was carried out using electrospray ionization(ESI)in both positive and negative ion modes using multipl e reaction monitoring(MRM).Matrix-matched external standard quantification was used.Results:Under the optimized conditions,the 30 antiparasitic drugs showed good linearity within their respective linear ranges,with coefficient of determination(r^(2))greater than 0.99.The recoveries ranged from 70.1%to 111%,and the relative standard deviations were between 0.10%and 9.1%(n=6).The method detection limit rang ed from 0.001 to 0.3μg/kg,and the method quantification limit ranged from 0.004 to 1μg/kg.Conclusion:The method is sensitive,accurate,and exhibits good repeatability and stability,making it suitable for detecting various antiparasit ic drug residues in animal-derived food.