Development and validation of a sensitive solid-phase-extraction (SPE) method using high-performance liquid chromatography/tandem mass spectrometry (LC-MS/MS) for determination of risedronate concentrations in human plasma.
Summary of "Development and validation of a sensitive solid-phase-extraction (SPE) method using high-performance liquid chromatography/tandem mass spectrometry (LC-MS/MS) for determination of risedronate concentrations in human plasma."
Risedronate is a commonly prescribed bisphosphonate for the treatment of bone disorders. Due to its high polarity and low oral bioavailability, low concentrations of risedronate are expected in human plasma and therefore a sensitive assay is required to serve in pharmacokinetic studies. Here, we describe the development and validation of an LC-MS/MS assay for the measurement of risedronate concentrations in human plasma. Risedronate and the internal standard, risedronate-d4, were derivatized on an anion exchange solid-phase extraction cartridge. Trimethylsilyl-diazomethane which is a thermally stable and relatively non-toxic derivatization agent was used to methylate the risedronate phosphonic acid groups and decrease analyte polarity. Following extraction, the analytes were separated on a Phenomenex Gemini C18 column (150mm×2.0mm, 5μm), using a gradient of ammonium acetate 10mM and acetonitrile with a flow rate of 300μL/min. The assay calibration range was 0.2-25ng/mL. The calibration curve of risedronate standards spiked in six individual plasma samples was linear (r(2)=0.9998). Accuracy (percent deviation from nominal) and precision (percent coefficient of variation) at concentrations 0.5, 5 and 20ng/mL, and at the lower limit of quantification (LLOQ) of 0.2ng/mL were excellent at <6%. Mean recovery was 54% for risedronate and 51% for the internal standard. Risedronate was stable in human plasma samples for at least 5h at room temperature, 101 days frozen at -80°C, 72h in an autosampler at 10°C, and for three freeze/thaw cycles. The validated assay method successfully quantified the concentrations of risedronate in plasma samples from informed consenting healthy volunteers administered a single 35mg risedronate tablet.
Affiliation
Centre for Integrated Preclinical Drug Development, The University of Queensland, Brisbane, QLD, Australia.
Journal Details
This article was published in the following journal.
Name: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
ISSN: 1873-376X
Pages: 34-41
Links
- PubMed Source: http://www.ncbi.nlm.nih.gov/pubmed/22197608
- DOI: http://dx.doi.org/10.1016/j.jchromb.2011.11.031
Medical and Biotech [MESH] Definitions
Solid Phase Extraction
An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods.
Analytic Sample Preparation Methods
Use of various chemical separation and extraction methods, such as SOLID PHASE EXTRACTION; CHROMATOGRAPHY; and SUPERCRITICAL FLUID EXTRACTION; to prepare samples for analytical measurement of components.
Chromatography, Gas
Fractionation of a vaporized sample as a consequence of partition between a mobile gaseous phase and a stationary phase held in a column. Two types are gas-solid chromatography, where the fixed phase is a solid, and gas-liquid, in which the stationary phase is a nonvolatile liquid supported on an inert solid matrix.
Gels
Colloids with a solid continuous phase and liquid as the dispersed phase; gels may be unstable when, due to temperature or other cause, the solid phase liquefies; the resulting colloid is called a sol.
Solid Phase Microextraction
A solventless sample preparation method, invented in 1989, that uses a fused silica fiber which is coated with a stationary phase. It is used for sample cleanup before using other analytical methods.
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