摘要
为建立并优化一种同位素-高效液相色谱-串联质谱法同时测定鸭蛋中4种硝基咪唑类药物(甲硝唑、地美硝唑、羟基甲硝唑、羟基地美硝唑)残留的检测方法,将样品经柠檬酸缓冲液和乙腈提取,超声波助提,平行蒸发仪减压浓缩后,用混合强阳离子固相萃取柱(MCX)净化。以Kinetex F5五氟苯基色谱柱分离,0.1%甲酸水和甲醇溶液为流动相进行梯度洗脱,在电喷雾离子源(ESI)正离子模式下,采用多反应监测模式(MRM)进行检测,以同位素内标法定量分析。结果显示:4种硝基咪唑类药物在0.5~200.0μg/L范围内线性关系良好,相关系数均大于0.997,加标回收率为90%-110%,相对标准偏差(RSDs)为4.76%~7.17%。结果表明,该方法回收率高、准确性好,可完全满足对4种硝基咪唑类药物残留检测的定性、定量需求,为食品中污染物监测提供了有效的技术支撑。
In order to establish a method to simultaneously determine drug residues of four nitroimidazoles(including metronidazole,dimetronidazole,hydroxy metronidazole and hy droxy dimetronidazole)in duck eggs using isotope high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS),samples,assisted by ultrasonic wave,were extracted with citric acid buffer and acetonitrile,concentrated under reduced pressure by a parallel evaporator,then purified using a mixed-mode cation exchanger(MCX)solid phase extraction(SPE)column.Using Kinetex F5 pentafluorophenyl chromatographic column for separation,gradient elution was conducted when 0.1%formic acid water and methanol solution were as mobile phases,then the drug residues were detected by a multi reaction monitoring mode(MRM)under the positive ion mode of electric spray ion source(ESI),and quantitatively analyzed by the isotope internal standard method.The results revealed that the linear relation of the four nitroimidazoles remained good within the range from 0.5 to 200.0μg/L,with the correlation coefficients above 0.997,standard recovery rates ranging from 90%to 110%,and relative standard deviations(RSDs)from 4.76%to 7.17%.In conclusion,the method,with high recovery rate and accuracy,could be effective enough to determine the drug residues of four nitroimidazoles qualitatively and quantitatively,providing a technical support for future monitoring of contaminations possibly contained in food.
作者
王圆圆
李宁
贾浩程
户瑞刚
曹玲芝
肖琎
Wang Yuanyuan;Li Ning;Jia Haocheng;Hu Ruigang;Cao Lingzhi;Xiao Jin(Tangshan Agricultural Comprehensive Administrative Law Enforcement Detachment,Tangshan,Hebei 063000,China;Zunhua Bureau of Agriculture and Rural Affairs,Zunhua,Hebei 064200,China;Tangshan Food and Drug Comprehensive Inspection and Testing Center,Tangshan,Hebei 063000,China;Tangshan Animal Quarantine Station,Tangshan,Hebei 063000,China;Hengshui Agricultural Comprehensive Administrative Law Enforcement Detachment,Hengshui,Hebei 053000,China)
出处
《中国动物检疫》
CAS
2023年第10期112-116,共5页
China Animal Health Inspection
基金
动物源性食品中多种药物残留检测技术研究与应用(22150220A)。
