Rapid communications in mass spectrometry : RCM
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Rapid Commun. Mass Spectrom. · Jan 2008
Determination of lopinavir and ritonavir in blood plasma, seminal plasma, saliva and plasma ultra-filtrate by liquid chromatography/tandem mass spectrometry detection.
A method based on liquid-liquid extraction followed by high-performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) detection was developed for the simultaneous determination of lopinavir (LPV) and ritonavir (RTV) in human blood, semen and saliva samples. The acquisition was performed in multiple reaction monitoring (MRM) mode, monitoring the transitions: m/z 629 > 447.1 for LPV, 721.18 > 268.02 for RTV and m/z 747.22 > 322.03 for the internal standard (IS). The limit of quantification was 1 ng/mL for both analytes in all matrices. ⋯ The extraction efficiencies were 73.5-118.4% for LPV and 74.4-126.2% for RTV. The analytical method was applied to measure LPV and RTV concentrations in blood plasma (total and unbound fraction), saliva and semen of six HIV+ individuals under stable treatment with Kaletra soft gel capsules. The results were consistent with previously published data.
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Rapid Commun. Mass Spectrom. · Jan 2008
A mass spectrometric method to simultaneously measure a biomarker and dilution marker in exhaled breath condensate.
Exhaled breath condensate (EBC) collection is a simple and non-invasive method to sample airway secretions, but analysis is limited by extensive and variable dilution of airway secretions within the condensate. To overcome this limitation, we developed a sensitive and specific liquid chromatography/tandem mass spectrometry (LC/MS/MS) method to simultaneously detect adenyl purines as biomarkers of inflammation and urea as a dilution marker in EBC. ⋯ Using these methods, we detected urea and the adenyl purines adenosine and AMP in EBC from seven subjects with cystic fibrosis (CF) and seven healthy controls and found that the AMP/urea ratio was elevated in the CF samples. These results demonstrate that mass spectrometry can be used successfully in EBC analysis to simultaneously detect a biomarker for airway inflammation and control for variable dilution.
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Rapid Commun. Mass Spectrom. · Jan 2008
Comparative StudyAn exploratory comparative study of volatile compounds in exhaled breath and emitted by skin using selected ion flow tube mass spectrometry.
Selected ion flow tube mass spectrometry (SIFT-MS) has been used to carry out a pilot parallel study on five volunteers to determine changes occurring in several trace compounds present in exhaled breath and emitted from skin into a collection bag surrounding part of the arm, before and after ingesting 75 g of glucose in the fasting state. SIFT-MS enabled real-time quantification of ammonia, methanol, ethanol, propanol, formaldehyde, acetaldehyde, isoprene and acetone. Following glucose ingestion, blood glucose and trace compound levels were measured every 30 min for 2 h. ⋯ The blood glucose increased to a peak about 1 h post-ingestion, but this change was not obviously correlated with temporal changes in any of the compounds in breath or emitted by skin, except for acetone. The decrease in breath acetone was closely mirrored by skin-emitted acetone in three volunteers. Breath and skin acetone also clearly change with blood glucose and further work may ultimately enable inferences to be drawn of the blood glucose concentration from skin or breath measurements in type 1 diabetes.
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Rapid Commun. Mass Spectrom. · Jan 2008
A selected ion flow tube mass spectrometry study of ammonia in mouth- and nose-exhaled breath and in the oral cavity.
A study has been carried out, involving three healthy volunteers, of the ammonia levels in breath exhaled via the mouth and via the nose and in the static oral cavity using on-line, selected ion flow tube mass spectrometry (SIFT-MS), obviating the problems associated with sample collection of ammonia. The unequivocal conclusion drawn is that the ammonia appearing in the mouth-exhaled breath of the three volunteers is largely generated in the oral cavity and that the ammonia originating at the alveolar interface in the lungs is typically at levels less than about 100 parts-per-billion, which is a small fraction of the total breath ammonia. This leads to the recommendation that exhaled breath analyses should focus on nose-exhaled breath if the objective is to use breath analysis to investigate systemic, metabolic disease.