Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples

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• 作者：Ning Liang ; Peiting Huang ; Xiaohong Hou ; Zhen Li…
• 关键词：Antibiotics ; Dispersive liquid ; liquid microextraction ; Solid ; phase extraction ; Ultra ; high performance liquid chromatography ; tandem mass spectrometry ; Water samples
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2016
• 出版时间：February 2016
• 年：2016
• 卷：408
• 期：6
• 页码：1701-1713
• 全文大小：2,313 KB
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• 作者单位：Ning Liang (1)
  Peiting Huang (1)
  Xiaohong Hou (1)
  Zhen Li (1)
  Lei Tao (2)
  Longshan Zhao (2)
  
  1. School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, Shenyang, Liaoning, 110016, China
  2. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning, 110016, China
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min−1, and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1–1000 ng mL−1 (sulfamethoxazole, cefuroxime axetil), 5–1000 ng mL−1 (tinidazole), 10–1000 ng mL−1 (chloramphenicol), 2-1000 ng mL−1 (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1–400 ng mL−1 (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL−1, respectively. The relative recoveries of the target analytes were in the range from 64.16 % to 99.80 % with relative standard deviations between 0.7 and 8.4 %. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results. Keywords Antibiotics Dispersive liquid-liquid microextraction Solid-phase extraction Ultra-high performance liquid chromatography-tandem mass spectrometry Water samples