鸡肉中多种抗生素超高效液相-静电场轨道阱高分辨质谱检测方法

Determination of antibiotic residues in chicken meat using ultra-highperformance liquid chromatography coupled with hybrid quadrupole-orbitrap high-resolution mass spectrometry

目的基于平行反应监测(PRM)模式的超高效液相-静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap-MS)法,通过优化样品前处理方法建立鸡肉中抗生素残留的检测方法。方法通过空白基质加标的鸡肉样品,采用含乙二胺四乙酸二钠和甲酸的95%乙腈水溶液提取;提取液采用C18、PSA和GCB 3种填料的不同组合方式净化并选择抗生素回收率较高的组合;采用UPLC-Q-Orbitrap-MS的PRM模式测定32种抗生素残留。结果采用C18填料净化提取液,加标回收率>80%的抗生素数量最多,基质效应为82.2%~112.6%。32种抗生素的检出限为0.8~5.8μg/kg,线性相关系数均>0.99,加标回收率为71.3%~111.5%,相对标准偏差为3.2%~14.2%。结论该方法适用于鸡肉中多种抗生素的检测与定量分析。

Objective To optimize the sample pretreatment and establish an ultra-high-performance liquid chromatogra⁃phy coupled with hybrid quadrupole-orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap-MS)assay based on the parallel reaction monitoring(PRM)mode for determination of antibiotic residues in chicken meat.Methods Blank matrix-spiked chicken meat samples were extracted with 95%acetonitrile aqueous solution containing Na2EDTA and for⁃mic acid.The extraction solutions were cleaned up using different combinations of C18,PSA and GCB fillers,and the combinations with a higher antibiotic recovery rate was screened.The residues of 32 antibiotics were determined using UPLC-Q-Orbitrap-MS based on the PRM mode.Results If the extraction solution was cleaned up using the C18 filler,the largest number of antibiotics with a spiked recovery rate of>80%was seen,with matrix effects of 82.2%to 112.6%.The detection limits of 32 antibiotics were 0.8 to 5.8μg/kg,with linear correlation coefficients of>0.99,spiked recovery rates of 71.3%to 111.5%and relative standard deviations of 3.2%to 14.2%.Conclusion The UPLCQ-Orbitrap-MS assay is suitable for determination and quantitative analysis of multiple antibiotics in chicken meat.