磁性固相萃取-高效液相色谱-串联质谱法测定环境水样中的四环素类抗生素  

Determination of tetracycline antibiotics in environmental water using magnetic solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry

作　　者：国明[1] 于峰[1] 贾科玲[1] 李姣[1] 孙海[1] 

机构地区：[1]浙江省化工研究院,浙江杭州310023

出　　处：《色谱》2016年第4期407-413,共7页Chinese Journal of Chromatography

基　　金：浙江省公益性技术应用研究(分析测试)项目(2014C37090)~~

摘　　要：建立了磁性固相萃取-高效液相色谱-串联质谱同时测定环境水样中四环素类抗生素的方法。以6种四环素类抗生素（差向四环素、土霉素、四环素、去甲金霉素、金霉素和脱水四环素）为目标化合物,考察并优化了吸附和解吸条件,确定了最佳萃取条件。萃取后的目标化合物经ZORBAX Eclipse Plus C18柱分离,用高效液相色谱-串联质谱在多反应监测（MRM）模式下进行检测。在优化的条件下,6种四环素在1~100μg/L范围内线性关系良好,线性相关系数为0.996 7~0.999 3,检出限为2.44~25.21 ng/L,样品加标回收率为80.6%~90.0%,日内相对标准偏差（RSDs）为0.6%~2.5%,日间RSDs为1.1%~7.1%。该方法灵敏度高、背景干扰低,适用于环境水样中6种痕量四环素类抗生素的同时检测。A method has been developed for the simultaneous determination of tetracycline antibiotics in environmental water by magnetic solid phase extraction and high performance liquid chromatography-tandem mass spectrometry. Several important parameters affecting the magnetic solid phase extraction procedure have been optimized for the best recovery. The eluate was analyzed by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/ MS）under multiple reaction monitoring（MRM）mode with a ZORBAX Eclipse Plus C18 column. Under the optimized conditions,the six tetracycline antibiotics（4-epitetracycline,oxytetracycline,tetracycline,demclocycline,chlortetracycline,anhydrotetracycline） showed good linearities in the range of 1-100 μg/L with the correlation coefficients of 0. 996 7-0. 999 3.The limits of detection（LODs）were in the range of 2. 44 ng/L to 25. 21 ng/L. The spiked recoveries were 80. 6%-90. 0%. The intra-day relative standard deviations（RSDs）were 0. 6%-2. 5%,while the inter-day RSDs were 1. 1%- 7. 1%. The method has low background and high sensitivity. It was successfully applied to the simultaneous determination of the six trace tetracycline antibiotics in environmental water.

关 键 词：磁性固相萃取 高效液相色谱-串联质谱 四环素类抗生素 环境水样 

分 类 号：O658[理学—分析化学]