Rapid quantification of miglustat in human plasma and cerebrospinal fluid by liquid chromatography coupled with tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Jan 15;877(3):149-54. doi: 10.1016/j.jchromb.2008.11.040. Epub 2008 Dec 3.

Abstract

Miglustat (OGT 918) is an iminosugar recently introduced in therapeutic as potential alternative therapy in disorders found in several diseases such as Tay-Sachs, Gaucher or Niemann-Pick diseases. A highly sensitive liquid-chromatography-electrospray tandem mass spectrometry (LC-MS/MS) assay was developed for the quantification of miglustat in human plasma and cerebrospinal fluid (CSF). The sample preparation consists in a simple protein precipitation with a mixture of acetonitrile/methanol (75/25) which yields 100% recovery. The isocratic separation utilizes an Atlantis Hilic (3 microm, 150 mm x 2.1 mm) column, with a mobile phase of acetonitrile/water/ammonium acetate buffer (75/10/15, v/v/v) delivered at 230 microl/min. Selected reaction monitoring (SRM) mode was used with the transitions m/z 220-->158 for the miglustat and m/z 208-->m/z 146 for the miglitol (internal standard). Good linearity was observed in a range from 125 to 2500 ng/ml and from 50 to 1000 ng/ml, for plasma and CSF, respectively. The within-run precision of the assay was less than 6%, and the between-run run precision was less than 6.5%, for six replicates at each of three concentrations and evaluated on three separated days for both plasma and CSF mediums. Assay accuracy was in the range of 98-106.5%. Stability of miglustat was reported under a variety of storage conditions. The miglustat concentrations in two children are presented to demonstrate the clinical interest of this new method.

MeSH terms

  • 1-Deoxynojirimycin / analogs & derivatives*
  • 1-Deoxynojirimycin / analysis
  • 1-Deoxynojirimycin / blood
  • 1-Deoxynojirimycin / cerebrospinal fluid
  • Calibration
  • Child
  • Chromatography, Liquid*
  • Drug Stability
  • Enzyme Inhibitors / blood*
  • Enzyme Inhibitors / cerebrospinal fluid*
  • Humans
  • Least-Squares Analysis
  • Reference Standards
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry* / methods

Substances

  • Enzyme Inhibitors
  • miglitol
  • 1-Deoxynojirimycin
  • miglustat