4.8 Article

Fully Automatic Sample Treatment by Integration of Microextraction by Packed Sorbents into Commercial Capillary Electrophoresis-Mass Spectrometry Equipment: Application to the Determination of Fluoroquinolones in Urine

期刊

ANALYTICAL CHEMISTRY
卷 81, 期 8, 页码 3188-3193

出版社

AMER CHEMICAL SOC
DOI: 10.1021/ac900234j

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资金

  1. Spanish Ministry of Innovation and Science [CTQ2007-60426]
  2. Junta of Andalusia [FQM02300]
  3. Ministry for the award of a Research Training Fellowship [BES-2005-10603]

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This paper describes a new and innovative way to integrate microextraction by packed sorbents (MEPS) into commercial CE equipment. The suggested integration allows the automatic sample cleanup and preconcentration requiring only a few microliters of sample and no additional hardware and software. The MEPS was integrated in the outlet region of a commercial CE equipment cartridge in order to provide easy manipulation and exchange. The robustness of the proposed integration was demonstrated by the design and use of a (MEPS)-nonaqueous capillary electrophoresis (NACE)-MS method used to determine fluoroquinolones FQs (namely, ofloxacin, marbofloxacin, enrofloxacin, danofloxacin, and difloxacin) in urine. The method allows the analysis of micrograms per liter of FQs to be carried out with only 48 mu L of urine sample. The obtained LODs were in the range 6.3-10.6 mu g/L. An analysis of spiked urine samples was used to validate the method. Absolute recoveries were in the range of 71-109% while the precision expressed as repetitivity of peak area was lower than 5.9%.

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