172023,Vol.37,No.7分析检测肉类研究MEATRESEARCH中国肉类食品综合研究中心CHINAMEATRESEARCHCENTER超高效液相色谱-串联质谱法检测禽畜肉中头孢曲松钠药物残留黄美玲（广电计量检测（福州）有限公司，福建福州350001）摘要：建立超高效液相色谱-串联质谱法测定禽畜肉中头孢曲松钠药物残留量的方法。禽畜肉样品经乙腈-水溶液（8∶2，V/V）振荡涡旋，超声提取，QuEChERS法净化，通过BEHC18色谱柱进行分离，以0.1%甲酸和甲醇为流动相，采用多反应监测模式分析，电喷雾离子源正离子模式（ESI＋）扫描，外标法定量。结果表明：头孢曲松钠线性关系良好，相关系数（R2）大于0.999；检出限为3.0μg/kg，定量限为9.0μg/kg；头孢曲松钠在不同禽畜肉基质中进行高、中、低3种添加水平的回收率实验，平均加标回收率为87.17%～105.21%，相对标准偏差为3.14%～6.13%。该方法简单、快捷、灵敏、准确、可操作性强，适用于监管机构快速检测禽畜肉中头孢曲松钠残留量。关键词：超高效液相色谱-串联质谱法；头孢曲松钠；禽畜肉；QuEChERSDetectionofCeftriaxoneSodiumResidueinLivestockandPoultryMeatbyUltra-PerformanceLiquidChromatography-TandemMassSpectrometryHUANGMeiling(GRGMetrologyandTestFuzhouCo.Ltd.,Fuzhou350001,China)Abstract:Inthisstudy,ananalyticalmethodforthedeterminationofceftriaxonesodiumresiduesinmeatusingultra-performanceliquidchromatography-tandemmassspectrometry(UPLC-MS/MS)wasestablished.Thesampleswerehomogenizedwithacetonitrile-water(8:2,V/V)usingavortexmixerandultrasonicallyextracted,andtheextractwascleanedupbythequick,easy,cheap,effective,ruggedandsafe(QuEChERS)method,andseparatedonaBEHC18columnusingamobilephaseconsistingof0.1%formicacidandmethanol.Theanalysiswasperformedundermultiplereactionmonitoring(MRM)inthepositiveelectrosprayionization(ESI+)mode.Theexternalstandardmethodwasusedforquantification.Theresultsshowedthatthecalibrationcurveforceftriaxonesodiumhadgoodlinearity,withacorrelationcoefficientgreaterthan0.999.Thedetectionlimitwas3.0μg/kg,andthequantificationlimitwas9.0μg/kg.Theaveragerecoveriesfordifferentmatricesspikedatthreeconcentrationlevelswere87.17%–105.21%withrelativestandarddeviations(RSDs)rangingfrom3.14%to6.13%.Thismethodis...
