固相萃取-高效液相色谱-串联质谱法测定畜禽肉中3种抗生素残留量  

Determination of the residues of 3 kinds of antibiotics in livestock and poultry meat by solid phase extraction high performance liquid chromatography-mass spectrometry

作　　者：乔庆东[1] 吴云钊[1] 庄景新[1] 曹民[1] 张晨[1] 孙潇 QIAO Qing-dong;WU Yun-zhao;ZHUANG Jing-xin;CAO Min;ZHANG Chen;SUN Xiao(Physical and Chemical Laboratory,Changping District Center for Disease Control and Prevention,Beijing 102200,China)

机构地区：[1]北京市昌平区疾病预防控制中心理化检验科,北京102200

出　　处：《中国卫生检验杂志》2022年第5期536-539,543,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立固相萃取-高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定畜禽肉产品中金霉素、土霉素和四环素3种抗生素的检测方法。方法样品经EDTA-Mcllvaine缓冲溶液超声提取,高速冷冻离心10 min(4℃,10000 r/min),滤液经正己烷脱脂,ProElut PLS固相萃取柱净化,氮气吹至近干。Shim-pack XR-ODSⅢ柱(50 mm×2.0 mm,1.6μm)色谱分离,流动相为0.2%甲酸水溶液-乙腈,梯度洗脱,流速为0.3 ml/min,进样量为10μl,柱温为40℃。多反应监测模式(MRM)测定,外标法定量。结果3种抗生素在25.0μg/L~400.0μg/L线性良好,相关系数(r>0.998);方法检出限为0.5μg/kg,3个加标水平的回收率在72.4%~94.3%,相对标准偏差(RSD)在3.2%~13.6%。结论该方法简便快速、灵敏可靠、干扰少、成本较低、重现性好,适用于畜禽肉产品中3种抗生素药物残留的同时测定。Objective To establish a method for the determination of aureomycin,oxytetracycline and tetracycline in livestock and poultry meat by ultrahigh performance liquid chromatography coupled with electrospray tandem mass spectrometry(UPLC-MS/MS).Methods The samples were pretreated with EDTA-Mcllvaine buffer solution as extraction agent,then centrifuged by high speed freezing centrifuge(10 min,4℃,10000 r/min).The filtrate was defatted withn-hexane,and further purified with ProElut PLS SPE column.The chromatographic separation was performed on a Shim-pack XR-ODSⅢcolumn(50 mm×2.0 mm,1.6μm)with mobile phase consisted of 0.2%formic acid aqueous solution-acetonitrile with gradient elution at the flow rate of 0.3 ml/min.The sample size was 10μl and the column temperature was 40℃.Multiple response monitoring mode(MRM)was used for determination,and external standard method for quantification.Results The method showed good linearity(r>0.998)in the range of 25.0μg/L-400.0μg/L.The detection limit of the method was 0.5μg/kg,theRSDs were 72.4%-94.3%and the recoveries were 3.2%-13.6%at three spiked levels.Conclusion The method is simple,rapid,sensitive and reliable.It is suitable for simultaneous determination of three antibiotic residues in livestock and poultry meat products.

关 键 词：固相萃取 高效液相色谱-串联质谱法 畜禽肉 四环素类 

分 类 号：O657.63[理学—分析化学]