Analysis of liver tissue for olestra following long-term feeding to rats and monkeys.

The potential for olestra to be absorbed and to accumulate in tissues was investigated by analysing liver tissue from rats and monkeys in long-term feeding studies using sensitive chromatographic methods. Studies with intravenously administered olestra indicated that absorbed olestra is predominantly taken up by the liver. In monkeys, 74% of the injected dose was detected in the liver, as intact olestra, 48 hr after dosing.

Long-term performance of a gas chromatography/tandem mass spectrometry assay for tebufelone in plasma.

An automated gas chromatography/tandem mass spectrometry (GC/MS/MS) based method for the rapid determination of tebufelone (TE) in animal and human plasma has been routinely applied in our laboratory to more than 3000 samples over a 2-year period. The selectivity of MS/MS conducted on a triple quadrupole instrument, combined with the use of a stable-isotope-labeled internal standard, results in excellent analytical figures of merit, as well as minimal sample preparation, rapid analysis, and high assay reliability. The work described here goes beyond initial method development and validation studies by evaluating the long-term performance of quantitative GC/MS/MS.

Determination of total and encapsulated insulin in a vesicle formulation.

A method for the determination of the amount of insulin in a vesicle formulation was developed. Samples were treated with anion exchange resin to quantitatively remove the insulin outside the vesicle walls. Encapsulated insulin was released from vesicles by disruption with a surfactant and the amount released was determined by reversed-phase HPLC.

Quantitation of vitamin B6 in biological samples by isotope dilution mass spectrometry.

Methods have been developed for the simultaneous quantitative analysis of vitamin B6 forms in biological samples by isotope dilution mass spectrometry using deuterated forms of pyridoxine, pyridoxal, pyridoxamine, and pyridoxic acid. The biological fluid or tissue sample was homogenized and then treated with a cocktail containing appropriate amounts of each deuterated vitamer, as well as the deuterated, phosphorylated vitamer forms. The individual vitamers were isolated from the homogenate by a complex high-performance liquid chromatographic procedure that provided separate fractions for each of the six vitamers found in biological samples.