PubMed · 15418549
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V L LINDBERG. A calibrated light separator.. https://pubmed.ncbi.nlm.nih.gov/15418549/
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A sensitive liquid chromatographic-tandem mass spectrometry(LC-MS/MS) method was developed for the determination of rizatriptan in human plasma. The analytes were extracted from plasma samples by liquid-liquid extraction, separated on a Zorbax XDB C8 column (150 x 4.6 mm i.d.) and detected by tandem mass spectrometry with an electrospray ionization interface. Zomitriptan was used as the internal standard. The method had a lower limit of quantitation of 50 pg/mL for rizatriptan, which showed more sensitivity and speed of analysis compared with reported methods. The within- and between-day precision was measured to be below 11.71% and accuracy between -5.87 and 0.86% for all quality control samples. This quantitation method was successfully applied to the evaluation of the pharmacokinetic profiles of rizatriptan after single oral administration of 5, 10 and 15 mg rizatriptan tablets to 10 healthy volunteers (five males and five females).
The potential for developing improved procedures for phosphate measurement through combinations of gel electrophoresis and quadrupole-based ICP mass spectrometry utilising (47)PO(+) is investigated. Laser ablation of gels offers a rapid and direct quantitation route, but is subject to high blanks due to P impurities in gels and associated reagents; nevertheless optimisation of laser sampling afforded improved method sensitivity (limit of detection 0.09 microg g(-1)). Implementation of whole gel elution (WGE) with FI-ICP-MS (conventional solution nebulisation) following gel electrophoresis permitted quantitation at the sub microg l(-1) level, and microcolumn processing (activated alumina) was effective at rejecting phosphate contamination. The potential for S-induced molecular ion interference at mass 47 was demonstrated.
Sulfur dioxide (SO(2)) is used as a preservative and stabilizer in wine production to prevent undesired biochemical processes in the must and the final product. The concentration of SO(2) is restricted by national regulations. There are two main forms of SO(2) in wine-free (inorganic forms) and bound (fixed to organic compounds, e.g. aldehydes). Iodometric titration is commonly employed for determination of SO(2) concentration (either by direct titration or after pre-separation by distillation); other techniques are also used. In this work inductively coupled plasma-optical-emission spectrometry with vapour generation was used for determination of free and total SO(2) in wine. Gaseous SO(2) is released from the sample by addition of acid and swept into the ICP by an argon stream. The intensity of the sulfur atomic emission lines is measured in the vacuum UV region. Determination of total SO(2) is performed after hydrolysis of bound forms with sodium hydroxide (NaOH). Concentrations of acid for vapour generation and NaOH for hydrolysis were optimised. The method was used for determination of free and total SO(2) in red and white wine samples and results were compared with those from iodometric titration.