Comparison of atmospheric pressure photoionization and ESI for CZE-MS of drugs.

The performance of atmospheric pressure photoionization (APPI) and ESI for CZE was compared using a set of seven drugs (basic amines, quaternary amines and steroids) and four different BGEs. The influence of volatile and nonvolatile BGEs of acidic and neutral pH on the MS responses of test compounds was evaluated by infusion of test solutions into the respective ion sources, and by actual CZE-MS experiments. The infusion experiments indicate that sodium phosphate buffers cause ionization suppression in ESI-MS, although for the amines the suppression was modest (25-60% signal reduction).

On-line coupling of SPE and CE-MS for peptide analysis.

An on-line SPE-CE-MS system has been developed for the analysis of peptides. Analytes are preconcentrated using a C(18) microcolumn (5 x 0.5 mm id), and then introduced into the CE system via a valve interface.

Analysis of recombinant human growth hormone by capillary electrophoresis with bilayer-coated capillaries using UV and MS detection.

The characterization of recombinant human growth hormone (rhGH; somatropin) by capillary electrophoresis (CE) with UV-absorbance and mass spectrometric (MS) detection using capillaries noncovalently coated with polybrene (PB) and poly(vinyl sulfonic acid) (PVS) is demonstrated. Compared with bare fused-silica capillaries, PB-PVS coated capillaries yielded more favorable migration-time reproducibilities and higher separation efficiencies. Optimal separation conditions for the bilayer-coated capillaries comprised a background electrolyte (BGE) of 400 mM Tris phosphate (pH 8.

Capillary electrophoresis-mass spectrometry of proteins at medium pH using bilayer-coated capillaries.

The feasibility of using noncovalently bilayer-coated capillaries for capillary electrophoresis-mass spectrometry (CE-MS) of acidic proteins was investigated using background electrolytes (BGEs) of medium pH. The capillary was coated by successively rinsing the capillary with solutions of the oppositely charged polymers polybrene (PB) and poly(vinyl sulfonic acid) (PVS). Volatile BGEs containing ammonium formate and/or N-methyl morpholine were tested at pH 7.

The use of perfusion scintigraphy to differentiate proximal right coronary artery stenosis from distal right coronary artery stenosis in patients with inferior left ventricular ischaemia.

Objective: The identification of patients with a significant proximal right coronary artery (RCA) is of clinical relevance since it may direct diagnostic and therapeutic strategies. This study was performed to determine parameters of (201)Tl RV perfusion SPECT which can be used to discriminate between proximal and distal RCA stenosis in patients with inferior left ventricular (LV) ischaemia. In addition, feasibility and reproducibility of a new semi-quantitative method for the assessment of RV perfusion were evaluated.

Direct sample injection for capillary electrophoretic determination of organic acids in cerebrospinal fluid.

Organic acids in cerebrospinal fluid (CSF) are potential diagnostic markers for neurological diseases and metabolic disorders. A capillary electrophoretic (CE) method for the direct analysis, i.e.

Coupling of sequential injection analysis and capillary electrophoresis - Laser-induced fluorescence via a valve interface for on-line derivatization and analysis of amino acids and peptides.

The on-line coupling of sequential injection analysis (SIA) and capillary electrophoresis (CE) via an in-line injection valve is presented. The SIA system is used for automated derivatization of amino acids and peptides. Dichlorotriazinylaminofluorescein serves as the derivatization agent, thus enabling sensitive laser-induced fluorescence detection of the derivatized analytes.

Micellar electrokinetic chromatography-electrospray ionization mass spectrometry for the identification of drug impurities.

Previously, we have presented a system hyphenating continuous micellar electrokinetic chromatography (MEKC) with electrospray ionization mass spectrometry (ESI-MS). Here we evaluate this technique for its applicability in impurity profiling of drugs using galantamine and ipratropium as test samples. A background electrolyte (BGE) of 10mM sodium phosphate (pH 7.

Efficient and highly reproducible capillary electrophoresis-mass spectrometry of peptides using Polybrene-poly(vinyl sulfonate)-coated capillaries.

The potential of capillaries noncovalently coated with a bilayer of oppositely charged polymers for the analysis of peptides by CE-MS was investigated. Bilayer coatings were produced by subsequently rinsing fused-silica capillaries with a solution of Polybrene (PB) and poly(vinyl sulfonate) (PVS). The PB-PVS coating showed to be fully compatible with MS detection causing no ionization suppression or background signals.

Interlaboratory study of a NACE method for the determination of R-timolol content in S-timolol maleate: assessment of uncertainty.

Analyses of statistical variance were applied to evaluate the precision and practicality of a CD-based NACE assay for R-timolol after enantiomeric separation of R- and S-timolol. Data were collected in an interlaboratory study by 11 participating laboratories located in Europe and North America. General qualitative method performance was examined using suitability descriptors (i.

On-line coupling of size exclusion chromatography and capillary electrophoresis via solid-phase extraction and a Tee-split interface.

An on-line size exclusion chromatography (SEC)-solid-phase extraction (SPE)-capillary electrophoresis (CE) system using a Tee-split interface has been developed for the analysis of peptides in biological fluids. The SEC column fractionates the sample by molecular size and the low-molecular-weight fraction, which contains the peptides, is directed to a C(18) SPE microcolumn, where the peptides are trapped and concentrated. The SPE column is desorbed with 425 nL acetonitrile and the effluent is sent to the Tee-split interface, which hydrodynamically splits (1:40) the flow and, thus, allows appropriate injection of analytes into the CE system.

No-carrier-added versus carrier-added123I-metaiodobenzylguanidine for the assessment of cardiac sympathetic nerve activity.

Purpose: No-carrier-added (nca) MIBG is primarily associated with specific uptake (i.e. uptake-1 mechanism).

Ventricular mechanical dyssynchrony and resynchronization therapy in heart failure: a new indication for Fourier analysis of gated blood-pool radionuclide ventriculography.

In patients with decreased left ventricular ejection fraction and conduction disease, ventricular mechanical dyssynchrony has been demonstrated. To date, resynchronization by biventricular pacing is increasingly used since it improves ventricular function and exercise capacity in patients with heart failure. To optimize and evaluate the effect of resynchronization therapy and to identify patients who may benefit from biventricular pacing the assessment of left ventricular synchronicity is essential.

Evaluation of the sensitivity of miniaturized liquid chromatography-electrospray ionization-mass spectrometry for pharmaceutical analysis.

LC-ESI-MS is applied frequently in pharmaceutical analysis. The sample amount is generally not restricted, however with LC-ESI-MS, a lack of sensitivity may still be observed with standard-bore LC columns in isocratic mode. Therefore, it was investigated whether increased sensitivity could be achieved by using miniaturized LC-ESI-MS.

On-line coupling of cyclodextrin mediated nonaqueous capillary electrophoresis to mass spectrometry for the determination of salbutamol enantiomers in urine.

The usefulness of the on-line coupling of nonaqueous capillary electrophoresis (NACE) with electrospray ionization (ESI) mass spectrometry (MS) using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) was demonstrated for the enantioselective determination of low concentrations of salbutamol in human urine. After optimization of several parameters, such as sheath-liquid composition and flow rate, nebulizing gas pressure, CE counter-pressure and position of the CE capillary outlet, a limit of quantification of 18 and 20 ng/ml was obtained for salbutamol enantiomers. Moreover, the relative standard deviation values for repeatability at a concentration of 30 ng/ml were below 7% for both enantiomers.

Atmospheric pressure photoionization for enhanced compatibility in on-line micellar electrokinetic chromatography-mass spectrometry.

Atmospheric pressure photoionization (APPI) is presented as a novel means for the combination of micellar electrokinetic chromatography (MEKC) and mass spectrometry (MS). The on-line coupling is achieved using an adapted sheath flow interface installed on an orthogonal APPI source. Acetone or toluene is added as dopant to the sheath liquid to enhance analyte photoionization.

Noncovalently bilayer-coated capillaries for efficient and reproducible analysis of proteins by capillary electrophoresis.

The suitability of noncovalently bilayer-coated capillaries for the analysis of proteins by capillary electrophoresis (CE) at medium pH was investigated. Fused-silica capillaries were coated simply by successively flushing with a polybrene (PB) and a poly(vinyl sulfonate) (PVS) solution. A protein test mixture was used to evaluate the performance of the coated capillaries.

Influence of collimator choice and simulated clinical conditions on 123I-MIBG heart/mediastinum ratios: a phantom study.

Purpose: (123)I presents imaging problems owing to high-energy photon emission. We investigated the influence of collimators on (123)I-MIBG heart/mediastinum ratios (H/M ratios). Secondly, we assessed the influence on H/M ratios of different activity concentrations, simulating clinical conditions.

On-line capillary electrophoresis-mass spectrometry using dopant-assisted atmospheric pressure photoionization: setup and system performance.

The on-line coupling of capillary electrophoresis (CE) and mass spectrometry (MS) via atmospheric pressure photoionization (APPI) is demonstrated. To achieve CE-APPI-MS, an adapted coaxial sheath-flow interface was combined with an ion-trap mass spectrometer equipped with an APPI source originally designed for liquid chromatography-MS. Effective photoionization of test compounds was accomplished after optimization of several interface and MS parameters, and of the composition and flow rate of the sheath liquid.

Chromatographic preconcentration coupled on-line to capillary electrophoresis via a tee-split interface.

Solid-phase extraction (SPE) and capillary electrophoresis (CE) are on-line coupled via a Tee-split interface, which provides hydrodynamic injection of the SPE eluate by flow splitting. The interface allows sample preconcentration independently from the CE separation and prevents sample matrix and washing solvents from entering the separation capillary. The effect of the Tee-split interface on the CE efficiency was examined using enkephalin peptides as model compounds.

Vulnerability of myocardial collateral perfusion: the impact of episodic hypertension.

In patients with coronary artery disease, the presence of left ventricular hypertrophy secondary to hypertension is associated with an increased collateral development. A patient is described who was admitted for myocardial ischemia and severe hypertension. One day after admission, coronary angiography revealed a proximal chronic occlusion of the left anterior descending artery with an extensive collateral vascularization originating from the right and circumflex coronary arteries.

Chromatographic preconcentration coupled to capillary electrophoresis via an in-line injection valve.

A preconcentration-capillary electrophoresis (CE) system using a small precolumn in combination with an in-line injection valve is presented. The advantage of the present design is the ability to perform the sample preconcentration fully independently from the CE separation and to prevent sample matrix and washing solvents from entering the CE capillary. With a micro injection valve, sample could be effectively introduced into the CE system in an in-line fashion without seriously affecting the CE separation efficiency.

Comparison between tagged MRI and standard cine MRI for evaluation of left ventricular ejection fraction.

Global left ventricular function is a prognostic indicator and is used to evaluate therapeutical interventions in patients with heart failure. Regional left ventricular function can be determined with tagged MRI. Assessment of global left ventricular function using the tagging data may have additional clinical value without incurring extra scanning time, which is currently a limiting factor in cardiac imaging.