江汉大学学报(自然科学版) ›› 2017, Vol. 45 ›› Issue (3): 209-213.doi: 10.16389/j.cnki.cn42-1737/n.2017.03.003

• 化学 • 上一篇    下一篇

SPE-HPLC 法测定环境水样中3 种痕量抗生素的含量

谭芳1,孙凯2,宋威1,陈高艺1   

  1. 1. 江汉大学 光电化学材料与器件教育部重点实验室,化学与环境工程学院,湖北 武汉 430056;2. 武汉市武昌区环保局,湖北 武汉 430070
  • 出版日期:2017-06-28 发布日期:2017-06-30
  • 作者简介:谭芳(1973—),女,高级实验师,硕士,研究方向:仪器分析教学与科研。
  • 基金资助:
    湖北省教育厅科学技术研究项目(B2015237)

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

TAN Fang1,SUN Kai2,SONG Wei1,CHEN Gaoyi1   

  1. 1. Key Laboratory of Optoelectronic Chemical Materials and Devices of Ministry of Education,School of Chemistry and Enviromental Engineering,Jianghan University,Wuhan 430056,Hubei,China;2. Wuchang District Enviromental Protection Bureau of Wuhan,Wuhan 430070,Hubei,China
  • Online:2017-06-28 Published:2017-06-30

摘要: 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. 25~2 μg/mL,四环素0. 4~2 μg/mL,磺胺甲噁唑0. 04~2 μg/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. 01 μg/mL,定量限分别为0. 25、0. 40、0. 04 μg/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。

关键词: 固相萃取, 高效液相色谱, 四环素, 氧氟沙星, 磺胺甲噁唑

Abstract: 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 ultrapure water - 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.

Key words: solid phase extraction(SPE), high performance liguid chromatography(HPLC), tetracycline, ofloxacin;sulfamethoxazole

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