超高效液相色谱-电喷雾串联质谱法同时测定生菜中四环素类抗生素及其代谢产物  

Determination of tetracyclines and their metabolites in lettuce by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：陈莉 贾春虹[1] 张乙涵[2] 刘冰洁[1] CHEN Li;JIA Chun-Hong;ZHANG Yi-Han;LIU Bin-Jie(Institute of Plant and Environment Protection, Beijing Academy of Agriculture and Forestry Science, Beijing 100097, China;College of Resouree and Environment, Sichuan Agricultural University, Chengdu 611130, China)

机构地区：[1]北京市农林科学院植物保护环境保护研究所,北京100097 [2]四川农业大学资源环境学院,成都611130

出　　处：《食品安全质量检测学报》2018年第6期1247-1253,共7页Journal of Food Safety and Quality

基　　金：重点研发计划项目(2017YFD0800900;2017YFD0201700);国家自然基金项目(41101482);北京市自然基金项目(8122021)~~

摘　　要：目的建立超高效液相色谱-电喷雾串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定生菜中9种四环素类抗生素及其代谢产物的残留分析方法。方法生菜样品采用EDTA-Mcllvaine缓冲液与乙腈混合溶液提取,HLB固相萃取小柱净化,色谱分离选择ACQUITY UPLC BEH C18色谱柱,以乙腈和0.2%甲酸水溶液为流动相进行梯度洗脱,得到的分离效果较好。质谱采用电喷雾正离子电离、多反应监测模式检测。结果在0.01~0.5 mg/L范围内线性相关系数r2均大于0.99。仪器检出限为1.085~15.780μg/kg,方法的定量限为3.617~42.526μg/kg。在4个添加水平0.01、0.05、0.1和0.5 mg/kg下,除脱水四环素和差向脱水四环素(其回收率<40%)外,其余四环素类抗生素及代谢产物在蔬菜中的添加回收率在为63.4%~101.3%,相对标准偏差为2.52%~12.56%。结论该方法灵敏度高,净化效果好,可以用于蔬菜中四环素类抗生素及其代谢产物的残留分析。Objective To establish a method for simultaneous determination of tetracyclines （TCs） and their metabolites in lettuce by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The antibiotics were extracted by mixed solvent of acetonitrile and EDTA-Mcllvaine buffer solution, and separated and purified with HLB column. The ACQUITY UPLC BEH C18 chromatographic column was selected by chromatographic separation and the gradient elution was carried out with acetonitrile and 0.2% formic acid aqueous solution as mobile phase. The TCs were finally detected by UPLC-MS/MS with ESI（＋） ionization, and quantified with multiple reaction monitoring （MRM） mode. Results In the range of 0.01-0.5 mg/L, the linear relationships between the peak area and concentration of TCs and their metabolites were good （r^2〉0.99）. The limits of detection （LODs） were 1.085-15.780 μg/kg, while the limits of quantification （LOQs） were 3.617-42.526 μg/kg for TCs and their metabolites. At the 4 spiked levels of 0.01, 0.05, 0.1 and 0.5 mg/kg, the average recoveries of TCs and their metabolites were 63.4%-101.3%, with relative standard deviations （RSDs） of 2.52%-12.56% in vegetables, except the recoveries of ATC and EATC （〈40%）. Conclusion This method has high sensitivity and good purification effect, which is suitable for detecting residues of TCs and their metabolites in vegetables.

关 键 词：四环素类抗生素 代谢产物 超高效液相色谱.串联质谱法 蔬菜 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]