【摘要】 建立了一种超高压液相色谱(UPLC)快速测定环境水样中8种痕量四环素的方法。利用稀土金属镧作为螯合试剂与水样中的四环素形成疏水性螯合物,温度驱动[Bmim]PF6分散萃取富集目标物,采用超高压液相色谱进行分离,紫外检测器检测,并对实验条件进行了优化。在最佳条件下,8种四环素在一定质量浓度范围内呈良好线性,r2均大于0.99,检出限为0.03~5.79μg.L-1,定量下限为0.09~19.1μg.L-1。在河水、鱼塘水、养猪场废水中的加标回收率分别为63%~96%、59%~94%、55%~86%。北京地区环境水样的检测结果显示,在养猪场的废水中检出金霉素和差向金霉素,质量浓度分别为2.14、0.09μg.L-1;河水和鱼塘水中未检出。该方法可快速、便捷地检测环境水样中四环素。更多还原

【Abstract】 A confirmatory method using ultrahigh pressure liquid chromatography(UPLC) coupled with tunable ultraviolet detector(TUV) was developed for the determination of trace levels of tetracyclines,including chlortetracycline(CTC),doxycycline(DC),4-epitetracycline(ETC),4-epichlortetracycline(ECTC),4-epianhydrotetracycline(EATC),oxytetracycline(OTC),tetracycline(TC) and anhydrotetracycline(ATC),in environmental water samples.The rare earth metal La ions were used as chelating agent to form a hydrophobic complex compound with TCs.Temperature induced ionic liquids dispersive liquid-liquid microextraction(DLLME)was used to concentrate the target compound.Effects of experimental conditions,including the kinds and amounts of ionic liquids,heating temperature,time of complexation and extraction,concentration of Triton X-114 and pH value,on extraction efficiencies were investigated.Under the optimum conditions,the calibration curves were linear in the range of 1.0-200 μg·L-1 for ETC,TC,DC and ATC,and 0.1-200 μg·L-1 for ECTC,CTC and EATC,and 10-200 μg·L-1 for OTC,respectively,with correlation coefficients(r2) more than 0.99.The limits of detection(LODs) ranged from 0.03 μg·L-1 to 5.79 μg·L-1,and the limits of quantitation(LOQs) were in the range of 0.09-19.1 μg·L-1.The spiked recoveries of eight target compounds in river water,fishpond water and leaching water of the pig farm soil were achieved in the range of 63%-96%,59%-94% and 55%-86%,respectively.The investigation results of environmental water samples in Beijing showed that 2.14 μg·L-1CTC and 0.09 μg·L-1 ECTC were detected in waste water from hoggery and no target compounds were found in the river water and fishpond water samples.As a result,this method could be applied in the rapid and convenient determination of eight tetracycline antibiotics in real environmental water samples.更多还原