SPE-HPLC法测定环境水样中3种痕量抗生素的含量

Determination of Three Antibiotics Residue in Environmental Water Samples with SPE-HPLC

建立了一种固相萃取-高效液相色谱法同时测定水体中氧氟沙星、四环素、磺胺甲噁唑浓度。样品经固相萃取小柱富集净化、超纯水-乙腈(75∶25,体积比)洗脱后,用高效液相色谱-紫外检测器测定。检测波长λ为274 nm,柱温30℃,流动相为乙腈-磷酸水溶液(50∶50,体积比),采用梯度洗脱程序,实现了3种待测组分的基线分离,线性范围为氧氟沙星0.25~2μg/mL,四环素0.4~2μg/mL,磺胺甲噁唑0.04~2μg/mL。空白加标回收率范围分别为82.32%~94.86%。氧氟沙星、四环素、磺胺甲噁唑的检出限分别为0.04、0.25、0.01μg/mL,定量限分别为0.25、0.40、0.04μg/mL。该方法具有快速简便、灵敏高效等优点,可满足实际工作的需要。

The author established a solid phase extraction-high performance liquid chromatography(SPE-HPLC)method to determinate concentrations of ofloxacin,tetracycline,sulfamethoxazole in water. The samples were enriched with solid phase extraction column,after being eluted with ultrapurewater-acetonitrile(75∶25,volume ratio),the samples were determinated with high performance liquid chromatography-ultraviolet detector. In the conditions of detection wavelength λ = 274 nm,column temperature 30 ℃,mobile phase as acetonitrile-phosphoric acid aqueous solution(50∶50,volume ratio),the author used a gradient elution program to achieve the baseline separation of three kinds tested components. Linear range of ofloxacin was 0. 25~2 μg/mL,tetracycline was 0. 4 ~ 2 μg/mL,sulfamethoxazole was 0. 04~2 μg/mL. Blank spiked recoveries were 82. 32% ~94. 86%.Detection limits of ofloxacin,tetracycline,sulfamethoxazole were 0. 04,0. 25,0. 01 μg/mL respectively,quantitation limits were 0. 25,0. 40,0. 04 μg/mL,respectively. This method is simple,rapid,sensitive and efficient to meet the needs of practical work.