摘要
目的建立液相色谱-串联质谱测定牛奶中10种四环素类化合物的方法。方法待测抗生素包括:四环素(Tetracycline,TC)、强力霉素(Doxycycline,DC)、金霉素(Chlorotetracycline,CTC)、土霉素(Oxytetracycline,OTC)、4-差向四环素(4-epi-Tetracycline,4-epi-TC)、4-差向金霉素(4-epi-Chlorotetracycline,4-epi-CTC)、4-差向土霉素(4-epi-Oxytetracycline,4-epi-OTC)、米诺环素(minocycline,MNIO)、美他环素(Methacycline,MTC)、地美环素(Demecycline,DMC)。样品经缓冲溶液提取,乙醇促进沉淀,HLB小柱净化后使用液相色谱-串联质谱进行测定。结果四环素类药物在质量浓度2~100μg/L范围内线性关系良好,DC、MNIO、MTC检出限为0.6μg/kg,定量限为2μg/kg;其他7种药物检出限为0.3μg/kg,定量限为1μg/kg。10种四环素类药物加标回收率均在90.8%~118.0%,RSD均<10.5%。结论本实验建立的方法操作简单、便捷,准确率高,适用于牛奶中四环素类化合物的日常监测。
Objective To establish a liquid chromatography-tandem mass spectrometric assay for determination of 10 tetracycline compounds in milk.Methods Ten tetracycline compounds included tetracycline(TC),doxycycline(DC),chlorotetracycline(CTC),oxytetracycline(OTC),4-epi-tetracycline(4-epi-TC),4-epi-chlorotetracycline(4-epi-CTC),4-epi-oxytetracycline(4-epi-OTC),minocycline(MNIO),methacycline(MTC),demecycline(DMC).Following extraction,ethanol precipitation,purification with HLB reverse phase extraction columns,tetracycline compound samples were determined using liquid chromatography-tandem mass spectrometry.Results Tetracycline compounds showed a good linear relationship with mass concentrations of 2~100μg/L.The detection limit of DC,MNIO and MTC was 0.6μg/L,and the limit of quantitation was 2μg/L.The detection limit of other seven tetracycline compounds was 0.3μg/L,and the limit of quantitation was 1μg/L.The spiked recovery rate of ten tetracycline compounds was 90.8% to 118%,with relative standard deviations of <10.5%.Conclusion The established liquid chromatography-tandem mass spectrometry is simple,convenient and highly accurate for daily monitoring of tetracycline compounds in milk.
作者
曹伊楠
张昊
吉文亮
CAO Yi-nan;ZHANG Hao;JI Wen-liang(Jiangsu Provincial Center for Disease Control and Prevention,Jiangsu Nanjing 210009,China)
出处
《江苏预防医学》
CAS
2023年第2期136-140,共5页
Jiangsu Journal of Preventive Medicine
关键词
液相色谱-串联质谱法
四环素类化合物
牛奶
Liquid chromatography-tandem mass spectrometry
Tetracycline compound
Milk