摘要
目的建立超声辅助衍生—液相色谱串联质谱快速检测鱼肉中4种硝基呋喃类代谢物残留的方法。方法鱼肉样品经匀质后在超声波辅助下水解和衍生,样品离心后经HLB净化柱净化,正离子模式下通过多反应监测模式(MRM)测定、内标法定量。结果超声温度和时间对衍生反应有影响,当温度为50℃、反应时间为120 min时实验结果最优,4种硝基呋喃代谢物在0.25~25.00μg/kg范围内线性良好,相关系数r>0.9980,检出限0.002~0.050μg/kg、定量限为0.006~0.170μg/kg;在1.0μg/kg和10.0μg/kg的添加水平下,平均回收率为78%~115%,相对标准偏差(RSD)为0.77%~5.38%。结论借助超声辅助衍生和内标法定量可实现鱼肉样品中硝基呋喃类代谢物的快速、准确、高灵敏检测分析。
Objective To developed a rapid method for detecting residue of 4 nitrofuran metabolites in fish by ultrasonic wave assisted derivation-liquid chromatography tandem mass spectrometry.Methods Samples of fish were hydrolyzed and derived by ultrasonic wave assisted process after homogenization,and purified by HLB column after centrifugation,then the analytes were detected by multiple reaction monitoring(MRM)mode under positive ion electrospray(ESI),and quantified with internal standard method.Results The temperature and time of ultrasound had effect on derivative reaction.The results were optimal when temperature and reaction time was set at 50℃and 120 min,respectively.The linearity of the 4 nitrofuran metabolites was good within 0.25-25.00μg/kg,with the correlation coefficient of r>0.9980,the detection limit from 0.002 to 0.050μg/kg and the quantification limit within 0.006-0.170μg/kg.The average recover rate was 78%-115%,with the relative standard deviation(RSD)from 0.77%to 5.38%,at the spiked levels of 1.0μg/kg and 10.0μg/kg.Conclusions A rapid,accurate and high sensitive method is successfully developed for the analysis and determination of nitrofuran metabolites in fish samples with internal standard quantification after ultrasonic wave assisted process.
作者
王猛
王康康
杨雪丽
李菁
马鑫
WANG Meng;WANG Kang-kang;YANG Xue-li;LI Jing;MA Xin(The Center for Disease Control and Prevention of Xinjiang Uygur Autonomous Region,Urumqi,Xinjiang 830002,China)
出处
《疾病预防控制通报》
2020年第3期28-31,38,共5页
Bulletin of Disease Control & Prevention(China)
基金
新疆维吾尔自治区自然科学基金项目(2018D01C083)。
关键词
超声辅助衍生
液相色谱串联质谱
鱼肉
硝基呋喃代谢物
Ultrasonic wave-assisted derivation
Derivation-liquid chromatography tandem mass spectrometry
Fish sample
Nitrofuran metabolites
