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.
作者
乔庆东
吴云钊
庄景新
曹民
张晨
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)
出处
《中国卫生检验杂志》
CAS
2022年第5期536-539,543,共5页
Chinese Journal of Health Laboratory Technology
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
Solid phase extraction
High performance liquid chromatography-mass spectrometry
Livestock and poultry meat
Tetracyclines
作者简介
乔庆东(1983-),男,本科,副主任技师,主要从事理化检验工作。
