Simultaneous determination of flucloxacillin and ampicillin in human plasma by ultra performance liquid chromatography-tandem mass spectrometry and subsequent application to a clinical study in healthy Chinese volunteers

J Pharm Biomed Anal. 2012 Feb 5:59:157-61. doi: 10.1016/j.jpba.2011.09.024. Epub 2011 Oct 4.

Abstract

A novel method has been developed for the simultaneous determination of flucloxacillin and ampicillin in human plasma by ultra performance liquid chromatography combined with tandem mass spectrometry (UPLC-MS/MS). The plasma was treated by single step of protein precipitation (PPT) with acetonitrile. The chromatographic separation was performed with a mobile phase consisting of 10mM ammonium formate and acetonitrile (68:32, v/v). The analyses were carried out by multiple reaction monitoring (MRM) using the precursor-to-product combinations of m/z 454.1→160.3 (flucloxacillin), m/z 350.1→106.4 (ampicillin) and m/z 436.1→277.3 (IS). Validation results indicated that the lower limit of quantification (LLOQ) were both 0.2 μg/mL and both assay exhibited a linear range of 0.2-500 μg/mL. The intra-batch precision (R.S.D.) was less than 10.6% and inter-batch R.S.D. was less than 11.2%, while accuracy was with ±8% and ±9.9%, determined from QC samples for flucloxacillin and ampicillin. A rapid, sensitive and specific method for simultaneous quantifying flucloxacillin and ampicillin in human plasma have been devised and successfully applied to a clinic pharmacokinetic study.

Publication types

  • Clinical Trial
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Adult
  • Ampicillin / blood*
  • Ampicillin / pharmacokinetics
  • Anti-Bacterial Agents / blood*
  • Anti-Bacterial Agents / pharmacokinetics
  • Calibration
  • China
  • Chromatography, High Pressure Liquid / instrumentation
  • Chromatography, High Pressure Liquid / methods*
  • Drug Stability
  • Floxacillin / blood*
  • Floxacillin / pharmacokinetics
  • Humans
  • Limit of Detection
  • Linear Models
  • Reference Standards
  • Reproducibility of Results
  • Tandem Mass Spectrometry / instrumentation
  • Tandem Mass Spectrometry / methods*
  • Young Adult

Substances

  • Anti-Bacterial Agents
  • Floxacillin
  • Ampicillin