液相色谱-串联质谱测定水产品中残留硝基呋喃类药物含量  

High-performance liquid chromatography-tandem mass spectrometry for determination of nitrofuran antibacterial drugs in aquatic products

作　　者：梁希扬[1] 张林田[1] 罗惠明[1] 张冬辉[1] 陈建伟[1] 

机构地区：[1]汕头出入境检验检疫局,广东汕头515041

出　　处：《中国卫生检验杂志》2007年第11期1986-1988,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立高效液相色谱-串联质谱仪测定水产品中残留硝基呋喃类药物含量。方法：样品经0.2M HCl提取,样品中的残留物与衍生化试剂2-硝基甲醛（NBA）反应,分别生成代谢产物NP-AOZ、NP-SEM、NP-AHD、NP-AMOZ,再经乙酸乙酯萃取,萃取液用氮气流挥干,残渣用乙腈-乙酸混合物溶解后用正己烷脱脂,用液相色谱-串联质谱仪测定。结果：各标准曲线相关系数均≥0.996,各成分在0.5、0.75、1.0μg/kg浓度水平加标回收率在76.8%～132.4%之间,RSD均≤13.9%。检测低限均为0.5μg/kg。结论：本法准确、简便、快速,具有良好的重现性和准确性,可用于水产品中残留硝基呋喃类药物含量的测定。Objective ：To develop a new method for the determination of nitrofuran antibacterial drugs in aquatic products by high- perforumnce liquid chromatography- tandem mass spectrometry. Methods：Drug residues in samples were extracted with 0. 2 moL/L HCI, reacted with derivative reagent 2 - NBA to obtain metabolized products - NP - AOZ, NP - SEM, NP - AHD and NP - AMOZ. These products were extracted with Ethyl Acetate and dried with nitrogen flow. After dissolved with acetate and - acetic -acid mixture and defatted with n -Hexane, the residues were then determinated by high -performance liquid chromatography -tandem mass spectrometry. Results：All the calibration curve＇s correlation coefficients were ≥0. 996. The average recoveries of 0. 5,0. 75,1.0 μg/kg were in the range of 76. 8% ~ 132.4% , with RSD ≤ 13.9% , the limit of detection of all these compounds was as low as 0. 5 txg/kg. Conclusion ：The method is validated with respect to simplicity, sensitivity, accuracy, good repeatability and reproducibility, All of the analytical results are conformed to the the deterumination of nitrofuran antibacterial drugs in aquatic products.

关 键 词：高效液相色谱-串联质谱 水产品 硝基呋喃类代谢物 

分 类 号：O657.63[理学—分析化学]