Are there published methods available for the LC-MS-MS analysis ofBack to the Top
these 2 beta blockers?
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This should help.
Clin Chem. 1985 Jan;31(1):131-4.
Assay of total and free propranolol in plasma by liquid chromatography
with fluorometric detection.
Ray K, Trawick WG, Mullins RE.
We report a liquid-chromatographic method for assay of total and free
propranolol and its metabolite, propranolol glycol, in plasma. An
ultrafiltration device is used to separate the free drugs from the
protein-bound drugs. The total and free drugs are isolated from plasma
or ultrafiltrate by liquid-solid extraction on a Waters C18 SEP-PAK and
the drugs are quantified on a C18 mu-Bondpak radial-compression column.
The mobile phase consists of equal parts of methanol and a solution of
potassium 50 mmol/L phosphate and 2.5 mmol/L 1-pentane-sulfonic acid,
pH 5.0. Detection was by fluorescence, with excitation at 296 nm and
emission at 338 nm. Time required for sample preparation for
total-propranolol assay is 40 min per eight samples. Sample preparation
for free-propranolol assay requires an additional 1 h per eight
samples. Chromatography requires 15 min per sample. The extraction
recovery is approximately 75% and the assay curve is linear from 5 to
400 micrograms/L. The run-to-run CV is 4% for total propranolol, 15%
for free propranolol.
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A high sensitivity reversed-phase HPLC method for the simultaneous
determination of marker compounds of paracellular transport (atenolol),
transcellular transport (propranolol) and P-gp functionality (talinolol)
J Pharm Biomed Anal. 2004 Mar 10;34(5):971-8.
HPLC with programmed wavelength fluorescence detection for the
determination of marker compounds of integrity and P-gp functionality
Caco-2 intestinal absorption model.
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