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0.9967～0.9993，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 liq-uid chromatography-tandem mass spectrometry. Several important parameters affecting the magnetic solid phase extraction procedure have been optimized for the best recovery. The elu-ate 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 tetra-cycline antibiotics in environmental water.
参考文献
| [1] | Patyra, E.;Kowalczyk, E.;Kwiatek, K..Development and validation method for the determination of selected tetracyclines in animal medicated feedingstuffs with the use of micellar liquid chromatography[J].Analytical and bioanalytical chemistry,201321(21):6799-6806. |
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