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Sensitive determination of ambenonium chloride in serum from patients with myasthenia gravis using ion-exchange resin extraction and reversed-phase ion-pair chromatography.

An effective and selective procedure for the extraction of ambenonium chloride (AMBC) from serum using a weak cation-exchange extraction cartridge has been developed. The solid-phase extraction procedure permitted the extraction of AMBC from serum without adhesion to materials such as the containers. A 200-microliter volume of the eluate could be directly injected on to a reversed-phase ion-pair high-performance liquid chromatographic column. The recovery was in the range 97-100%. The limit of detection for AMBC was 0.5 ng/ml in serum (signal-to-noise ratio = 3). The method was used to determine the serum concentration of AMBC in patients with myasthenia gravis. The method would be useful for monitoring AMBC in serum in order to study its pharmacokinetic behaviour in patients under oral administration therapy.

Adult↗

Radium-228 determination of natural waters via concentration on manganese dioxide and separation using Diphonix ion exchange resin.

The objective of this work was to establish a new procedure for 228Ra determination of natural waters via preconcentration of radium on MnO2 and separation of its daughter, 228Ac, using Diphonix ion exchange resin. Following removal of potential interferences via passage through an initial Diphonix Resin column, the first daughter of 228Ra, 228Ac, is isolated by chromatographic separation via a second Diphonix column. A holding time of > 30 h for 228Ac ingrowth in between the two column separations ensures secular equilibrium. Barium-133 is used as a yield tracer. Actinium-228 is eluted from the second Diphonix Resin with 5 ml 1M 1-Hydroxyethane-1,1-diphosphonic acid (HEDPA) and quantified by addition of scintillation cocktail and LSC counting. Radium (and 133Ba) from the load and rinse solutions from the 2nd Diphonix column may be prepared for alpha spectrometry (for determination of 223Ra, 224Ra, and 226Ra) by BaSO4 microprecipitation and filtration. Decontamination tests indicate that U, Th, and Ra series nuclides do not interfere with these measurements, although high contents of 90Sr (90Y) require additional treatment for accurate measurement of 228Ra. Addition of stable Sr as a "hold back" carrier during the initial MnO2 preconcentration step was shown to remove most 90Sr interference.

Chromatography, Ion Exchange↗