QuEChERS-UPLC-MS/MS法测定水产品中孔雀石绿和酰胺醇类抗生素残留量

Simultaneous determination of malachite green and amphenicols residues in aquatic products by QuEChERS-UPLC-MS/MS

建立了超高效液相色谱质谱联用法同时测定水产品肌肉组织中孔雀石绿和酰胺醇类抗生素残留的方法。样品经QuEChERS方法提取净化后,采用液相色谱-串联质谱测定,内标法定量。孔雀石绿(malachite green,MG)、隐色孔雀石绿(leucomalachite green,LMG)、氯霉素(chloramphenicol,CAP)和氟甲砜霉素(florfenicol,FF)在0.5~50.0 ng/mL质量浓度范围内线性良好(r≥0.9994)。甲砜霉素(thiamphenicol,TAP)在2.0~100.0 ng/mL质量浓度范围内线性良好(r≥0.9996)。MG、LMG、CAP和FF的检出限为0.1μg/kg,定量限为0.5μg/kg;TAP的检出限为0.4μg/kg,定量限为2.0μg/kg。MG、LMG、CAP和FF在0.5、2.0和10.0μg/kg加标水平时,加标回收率为72.0%~102.6%,精密度小于6.4%;TAP在2.0、10.0和50.0μg/kg加标水平时,其加标回收率为76.5%~95.4%,精密度小于5.1%。本方法适用于检测水产品中孔雀石绿类和酰胺醇类抗生素的残留,可为提升水产品质量安全水平提供技术支持。

An analytical method was established for the simultaneous determination of malachite green and amphenicols residues in the muscle tissues of aquatic products by ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS).The analytes were extracted and purified by QuEChERS,then determined by UPLC-MS,and quantified by internal standard method.The linearity of malachite green(MG),leucomalachite green(LMG),chloramphenicol(CAP)and florfenicol(FF)showed good in the range of 0.5~50.0 ng/mL(r≥0.9994),and that of thiamphenicol(TAP)was good in the range of 2.0~100.0 ng/mL(r<0.9996).The detection limits of MG,LMG,CAP and FF were 0.1μg/kg,respectively.The detection limits of TAP was 0.4μg/kg.The quantitative limits of MG,LMG,CAP and FF were 0.5μg/kg,respectively.The quantitative limits of TAP was 2.0μg/kg.The recovery of MG,LMG,CAP and FF was 72.0%~102.6%and the precision was less than 6.4%at 0.5,2.0 and 10.0μg/kg of internal standard.The recovery of TAP was 76.5%~95.4%and the precision was less than 5.1%at 2.0,10.0 and 50.0μg/kg of internal standard.In conclusion,this method is suitable for the detection of MG,LMG,CAP,FF and TAP residues in aquatic products,providing technological support for improving the quality and safety of aquatic products.