RP-HPLC法测定水体表层沉积物中的磺胺类与四环素类抗生素

Determination of Sulfonamides and Tetracyclines Antibiotics in Surface Sediments by Reversed Phase High Performance Liquid Chromatography

建立了超声提取-固相萃取/反相高效液相色谱检测水体表层沉积物中磺胺类和四环素类抗生素含量的方法。沉积物样品经冷冻干燥后用甲醇-EDTA/Mc Ilvaine缓冲液(1∶1)超声萃取,于40℃下氮气吹除提取液中有机溶剂后,过Poly-Sery HLB固相萃取小柱净化萃取,以ODS-P C_(18)反相色谱柱、紫外检测器进行色谱分析。结果表明:7种磺胺类抗生素在0.025~0.5 mg/L浓度范围内线性关系良好,相关系数(r2)均大于0.999,3个加标水平下的回收率为71.4%~107.6%,相对标准偏差(RSD,n=3)为1.4%~5.2%,方法检出限(MDL)为0.07~0.29 ng/g;3种四环素类抗生素在0.05~1 mg/L浓度范围内线性关系良好,r^2均大于0.999,3个加标水平下的回收率为62.2%~87.9%,RSD(n=3)为1.1%~4.6%,MDL为0.45~0.58ng/g。应用此方法对某城市湖泊及其引水河道表层沉积物进行检测,10种目标抗生素均被检出。该方法简单快速、精确可靠,适用于水体沉积物中磺胺类和四环素类抗生素的检测。

An ultrasonic extraction- solid-phase extraction -reversed phase high performance liquid chromatographic method was developed to determine sulfonamides and tetraeyclines antibiotics in sur- face sediments by optimizing condition of pretreatment. The sediment samples were extracted with a mixture of methanol - EDTA/MeIlvaine buffer（1 ： 1 ） under ultrasonieation after freeze-dried, then blowed at 40℃under nitrogen to remove the organic solvent. After purified with a Poly - Sery HLB solid-phase extraction cartridge, the extract was determined with ODS -P Cis column and UV -de- tector. The results showed that the calibration curves of 7 sulfonamides were the concentration range of 0. 025 - 0. 5 mg/L, and the recoveries of three sp 71.4% to 107.6% with relative standard deviations（RSDs, n = 3） of 1.4% linear （ r2 〉 0. 999 ） in iked levels ranged from - 5.2% . The method detection limits（MDL） ranged from 0. 07 ng/g to 0.29 ng/g. The calibration curves of 3 tetracy- elines were linear（r2 〉 0. 999） in the concentration range of 0. 05 - 1 mg/L, the recoveries at three spiked levels ranged from 62.2% to 87.9% , with RSDs（n = 3） of 1.1% -4.6% , and the method detection limits（MDL） were in the range of 0.45 -0. 58 ng/g. The developed method was applied to analyze the surface sediments of an urban lake and its inflowing rivers, in which 10 kinds of target antibiotics were all detected. The results showed that the method was simple, rapid and accurate, and was suitable to determine the sulfonamides and tetracyelines antibiotics in the sediments.