On-line coupling of solid-phase extraction to liquid chromatography-tandem mass spectrometry for the determination of macrolide antibiotics in environmental water

Anal Chim Acta. 2009 Feb 23;634(2):215-21. doi: 10.1016/j.aca.2008.12.022. Epub 2008 Dec 24.

Abstract

An automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) system was developed for the determination of macrolide antibiotics including erythromycin (ETM), roxithromycin (RTM), tylosin (TLS) and tilmicosin (TMC) in environmental water samples. A Capcell Pak MF Ph-1 column packed with restricted access material (RAM) was used as SPE column for the concentration of the analytes and clean-up of the sample. One milliliter water sample was injected into the conditioned SPE column and the matrix was washed out with 3 mL high purity water. By rotation of the switching valve, macrolides (MLs) were eluted in the back-flush mode and transferred to the analytical column by the chromatographic mobile phase. The matrix effect was evaluated by the directly injection LC-MS and on-line SPE-LC-MS methods. The limits of detection (LODs) and limits of quantification (LOQs) obtained are in the range of 2-6 and 7-20 ng L(-1), respectively, which means that the proposed method is suitable for trace analysis of MLs at low level concentration. The intra- and inter-day precisions are in the range of 2.9-7.2% and 3.3-8.9%, respectively. In the three fortified levels (20, 200 and 2000 ng L(-1)), recoveries of MLs ranging from 86.5% to 98.3% are obtained.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Anti-Bacterial Agents / analysis*
  • Calibration
  • Chromatography, Liquid / instrumentation
  • Chromatography, Liquid / methods
  • Macrolides / analysis*
  • Reproducibility of Results
  • Solid Phase Extraction / instrumentation
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / instrumentation
  • Tandem Mass Spectrometry / methods*
  • Time Factors
  • Water Pollutants, Chemical / chemistry*

Substances

  • Anti-Bacterial Agents
  • Macrolides
  • Water Pollutants, Chemical