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生态学杂志 ›› 2022, Vol. 41 ›› Issue (1): 190-198.doi: 10.13292/j.1000-4890.202201.002

• 技术与方法 • 上一篇    下一篇

液相色谱紫外-荧光串联检测器法检测我国污水中常见11种抗生素

曹君1,2,张雪娇1,赵青1,邢薇薇3,张思玉1*   

  1. 1中国科学院沈阳应用生态研究所, 沈阳 110016; 2中国科学院大学, 北京 100049; 3辽宁北方环境检测技术有限公司, 沈阳 110161)
  • 出版日期:2022-01-10 发布日期:2022-06-10

Determination of 11 antibiotics frequently detected in municipal wastewater in China by high-performance liquid chromatography with ultraviolet and fluorescence detector.

CAO Jun1,2, ZHANG Xue-jiao1, ZHAO Qing1, XING Wei-wei3, ZHANG Si-yu1*#br#   

  1. (1Institute of AppliedEcology, Chinese Academy of Sciences, Shenyang 110016, China; 2University of Chinese Academy of Sciences, Beijing 100049, China; 3Liaoning North Environmental Testing Technology Co. Ltd, Shenyang 110161, China).
  • Online:2022-01-10 Published:2022-06-10

摘要: 城市污水处理厂是环境中多种抗生素污染物的主要来源之一。建立污水中多种类抗生素的同时分析检测方法,可为获取该类污染物的常规监管提供技术储备。本研究以我国污水处理厂检出率最高的抗生素为目标污染物,建立了同时分析检测11种抗生素的高效液相色谱紫外/荧光检测器串联分析方法。该方法首先使用紫外检测器,在一组优化仪器参数条件下,实现11种目标物和内标物的完全分离检出(R>1.5),同时可串联荧光检测器,使喹诺酮类抗生素获得更低的检出限。针对11种目标物,该方法的检出限为4.2~22.8 μg·L-1,定量限为5.1~56.4 μg·L-1,回收率为43.5%~102.8%。使用此方法对沈阳市某污水处理厂污水样品中的抗生素进行分析检测,进水中检出了磺胺二甲嘧啶、环丙沙星和诺氟沙星,浓度分别为440.9、2784.8和515.2 ng·L-1;出水中检出了环丙沙星和诺氟沙星,浓度为118.9和444.7 ng·L-1。该方法操作简单,耗时短,检测限低,适用于我国污水处理厂进、出水中抗生素的常规分析检测,具有很好的应用前景。

关键词: 抗生素, 污水处理厂, 同时检出, 高效液相色谱紫外/荧光串联检测器

Abstract: Municipal wastewater plant is an important source of antibiotics in the environment. Development of analytical methods for simultaneous determination of diverse antibiotics in municipal wastewater is crucial for monitoring and regulation of antibiotics. An analytic method based on highperformance liquid chromatography with ultraviolet and fluorescence detector was developed for simultaneously analyzing the presence of 11 antibiotics among four classes of antibiotics most frequently detected in wastewater treatment plants in China. Under a set of optimum analytic parameters, complete separation and detection of the 11 target antibiotics and an internal standard (R>1.5) were obtained by employing an ultraviolet detector. By employing tandem fluorescence detector, lower detection limits were obtained for fluoroquinolone antibiotics. Limits of detection for the 11 target antibiotics ranged from 4.19 to22.8 μg·L-1, quantitative limits fell within 5.1-56.4 μg·L-1, and recovery rates were 43.5%-102.8%. Sewage samples from inlet and outlet of a wastewater treatment plant in Shenyang were analyzed by such method. Sulfadiazine, ciprofloxacin, and norfloxacin were detected in the inlet samples, with concentrations of 440.9, 2784.8, and 515.2 ng·L-1, respectively. In the outlet samples, only ciprofloxacin and norfloxacin were detected, with concentrations of 118.9 and 444.7 ng·L-1, respectively. This method is convenient, time-saving, low in detection limit, and thus is suitable for regular analysis of antibiotics in wastewater treatment plants in China.

Key words: antibiotics, wastewater treatment plant, simultaneous detection, HPLC-UV/FLD.