Analysis of ciprofloxacin in low- and high-fat milk by high-performance liquid chromatography-mass spectrometry

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Abstract

The quantitative analysis of antibiotics in different matrices is of increasing importance in in vitro studies of food-drug interactions in the drug-development process. Our objective was to develop a new, rapid and simple solid-phase extraction method without protein precipitation followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) for analysis of ciprofloxacin in low- and high-fat milk. The HPLC-MS method (a single-quadrupole mass spectrometer equipped with an electrospray ion source was used as detector) was validated using a quinolone derivative, aripiprazole, as internal standard. A C 8 column and gradient elution with 0.02 m ammonium acetate solution (pH 2.5) and acetonitrile mixtures (flow rate 0.5 mL min -1 ) were used for HPLC separation. Various modes of detection (diode-array detection and MS detection in scanning and selected-ion monitoring modes) were compared for selectivity and sensitivity of quantitative analysis of ciprofloxacin. Use of selected- ion monitoring resulted in a 1600:1 signal-to-noise ratio which can be successfully applied to milk matrices resulting in a lower limit of detection of 0.4 ng mL -1 and a lower limit of quantification of 4.0 ng mL -1 . Recovery was 99.06 ± 0.15 and 98.57 ± 0.14% for low- and high-fat milk, respectively. The method enables analysis of the free, biologically available, amount of ciprofloxacin in in vitro simulation of milk-ciprofloxacin interaction studies.

Original languageEnglish
Pages (from-to)117-131
Number of pages15
JournalActa Chromatographica
Volume22
Issue number1
DOIs
Publication statusPublished - Mar 1 2010

Fingerprint

High performance liquid chromatography
Ciprofloxacin
Mass spectrometry
Fats
Drug interactions
Ions
Monitoring
Quinolones
Mass spectrometers
Ion sources
Chemical analysis
Signal to noise ratio
Diodes
Flow rate
Anti-Bacterial Agents
Derivatives
Detectors
Scanning
Recovery
Milk

Keywords

  • Ciprofloxacin
  • Liquid chromatography
  • Mass spectrometry
  • Milk
  • Solid-phase extraction

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

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title = "Analysis of ciprofloxacin in low- and high-fat milk by high-performance liquid chromatography-mass spectrometry",
abstract = "The quantitative analysis of antibiotics in different matrices is of increasing importance in in vitro studies of food-drug interactions in the drug-development process. Our objective was to develop a new, rapid and simple solid-phase extraction method without protein precipitation followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) for analysis of ciprofloxacin in low- and high-fat milk. The HPLC-MS method (a single-quadrupole mass spectrometer equipped with an electrospray ion source was used as detector) was validated using a quinolone derivative, aripiprazole, as internal standard. A C 8 column and gradient elution with 0.02 m ammonium acetate solution (pH 2.5) and acetonitrile mixtures (flow rate 0.5 mL min -1 ) were used for HPLC separation. Various modes of detection (diode-array detection and MS detection in scanning and selected-ion monitoring modes) were compared for selectivity and sensitivity of quantitative analysis of ciprofloxacin. Use of selected- ion monitoring resulted in a 1600:1 signal-to-noise ratio which can be successfully applied to milk matrices resulting in a lower limit of detection of 0.4 ng mL -1 and a lower limit of quantification of 4.0 ng mL -1 . Recovery was 99.06 ± 0.15 and 98.57 ± 0.14{\%} for low- and high-fat milk, respectively. The method enables analysis of the free, biologically available, amount of ciprofloxacin in in vitro simulation of milk-ciprofloxacin interaction studies.",
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AU - Pápai, K.

AU - Budai, M.

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AU - Antal, I.

AU - Klebovich, I.

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N2 - The quantitative analysis of antibiotics in different matrices is of increasing importance in in vitro studies of food-drug interactions in the drug-development process. Our objective was to develop a new, rapid and simple solid-phase extraction method without protein precipitation followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) for analysis of ciprofloxacin in low- and high-fat milk. The HPLC-MS method (a single-quadrupole mass spectrometer equipped with an electrospray ion source was used as detector) was validated using a quinolone derivative, aripiprazole, as internal standard. A C 8 column and gradient elution with 0.02 m ammonium acetate solution (pH 2.5) and acetonitrile mixtures (flow rate 0.5 mL min -1 ) were used for HPLC separation. Various modes of detection (diode-array detection and MS detection in scanning and selected-ion monitoring modes) were compared for selectivity and sensitivity of quantitative analysis of ciprofloxacin. Use of selected- ion monitoring resulted in a 1600:1 signal-to-noise ratio which can be successfully applied to milk matrices resulting in a lower limit of detection of 0.4 ng mL -1 and a lower limit of quantification of 4.0 ng mL -1 . Recovery was 99.06 ± 0.15 and 98.57 ± 0.14% for low- and high-fat milk, respectively. The method enables analysis of the free, biologically available, amount of ciprofloxacin in in vitro simulation of milk-ciprofloxacin interaction studies.

AB - The quantitative analysis of antibiotics in different matrices is of increasing importance in in vitro studies of food-drug interactions in the drug-development process. Our objective was to develop a new, rapid and simple solid-phase extraction method without protein precipitation followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) for analysis of ciprofloxacin in low- and high-fat milk. The HPLC-MS method (a single-quadrupole mass spectrometer equipped with an electrospray ion source was used as detector) was validated using a quinolone derivative, aripiprazole, as internal standard. A C 8 column and gradient elution with 0.02 m ammonium acetate solution (pH 2.5) and acetonitrile mixtures (flow rate 0.5 mL min -1 ) were used for HPLC separation. Various modes of detection (diode-array detection and MS detection in scanning and selected-ion monitoring modes) were compared for selectivity and sensitivity of quantitative analysis of ciprofloxacin. Use of selected- ion monitoring resulted in a 1600:1 signal-to-noise ratio which can be successfully applied to milk matrices resulting in a lower limit of detection of 0.4 ng mL -1 and a lower limit of quantification of 4.0 ng mL -1 . Recovery was 99.06 ± 0.15 and 98.57 ± 0.14% for low- and high-fat milk, respectively. The method enables analysis of the free, biologically available, amount of ciprofloxacin in in vitro simulation of milk-ciprofloxacin interaction studies.

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