摘要
目的建立高效液相色谱法(high-performance liquid chromatography,HPLC)定量测定水产品中四环素类残留量,同时采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)进行定性确证和定量检测。方法优化缓冲提取液浓度、固相萃取柱类型、色谱条件选择等测定环节。样品经柠檬酸缓冲液提取,固相萃取柱净化后,以液相色谱-紫外检测器进行定量检测,同时通过高效液相色谱-串联质谱仪进行定性和定量检测。结果四环素类目标物在10~200 ng/mL范围内线性良好(r>0.999),在10、50、100μg/kg3个水平上进行加标回收实验,回收率为76.0%~94.5%,相对标准偏差为3.9%~7.4%,高效液相色谱法检出限为5μg/kg,高效液相色谱-串联质谱法检出限为1μg/kg。结论该方法简便、稳定、准确,适合测定水产品中的四环素类残留量。
Objective To establish a method for the determination of tetracycline’s residues in aquatic products by high performance liquid chromatography(HPLC)and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The concentration of buffer extract,solid phase extraction column type and chromatographic condition selection were optimized.The samples were extracted with citric acid buffer,purified with solid phase extraction column,quantitatively detected by liquid chromatography-ultraviolet detector,and qualitatively and quantitatively detected by high performance liquid chromatography-tandem mass spectrometry.Results Tetracycline targets had good linearity in the range of 10-200 ng/mL(r>0.999).With 3 spiked concentrations of 10,50 and 100μg/kg,the average recoveries were 76.0%-94.5%,the relative standard deviation were 3.9%-7.4%,the detection limit of HPLC was 5 g/kg,and the detection limit of HPLC-MS/MS was 1 g/kg.Conclusion The method is simple,stable and accurate,suitable for the determination of tetracycline residues in aquatic products.
作者
吴学贵
王一晨
黄肖凤
韩惠芳
李小梅
WU Xue-Gui;WANG Yi-Chen;HUANG Xiao-Feng;HAN Hui-Fang;LI Xiao-Mei(Hainan Willtest Technology Co.,Ltd.,Chengmai 571924,China)
出处
《食品安全质量检测学报》
CAS
2020年第22期8334-8340,共7页
Journal of Food Safety and Quality
关键词
高效液相色谱法
高效液相色谱-串联质谱法
四环素
水产品
high performance liquid chromatography
high performance liquid chromatography-tandem mass spectrometry
tetracycline
aquatic products
