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T Catalano

Publications and source records attributed to T Catalano.

12 recordsLinked to original sources
PubMed2001

Comparison of drug substance impurity profiles generated with extended length columns during packed-column SFC.

The current study assesses the effect of extending column length during gradient packed column sub/supercritical fluid chromatography (PCSFC) experiments on the detection of known and unknown impurities in a drug substance sample. Quantitative drug substance impurity profiles were generated and compared using multiple column PCSFC and HPLC conditions. Also, chromatographic figures of merit were estimated and compared for components of a standard mixture during PCSFC experiments, which used one column, four columns, and six columns in series.

Chromatography, High Pressure Liquid↗
PubMed2000

Aspects of column fabrication for packed capillary electrochromatography.

Various parameters have been evaluated to develop a process for optimization of column manufacture for packed capillary electrochromatography (CEC). Spherisorb ODS-1 was packed into 75 microm I.D. capillaries to establish a standard set of packing conditions to afford high-performance columns free of voids. Numerous silica-based packing materials including porous and non-porous reversed-phase and ion-exchange phases were employed to evaluate the applicability of the standard conditions. Success of column manufacture and performance demonstrate a relationship to the colligative properties of the packing materials under the applied conditions. Frequently encountered difficulties arising from inadequate column conditioning and void formation in the packed bed are identified and discussed.

Electrophoresis, Capillary↗
PubMed1999

Evaluation of 1.5 microM reversed phase nonporous silica in packed capillary electrochromatography and application in pharmaceutical analysis.

Reversed-phase nonporous silica (RP-NPS) of 1.5 microm dp is employed to demonstrate rapid and efficient separations in packed capillary electrochromatography (CEC). Two methods for packing capillaries and two techniques to manufacture frits used to hold the packing in place are evaluated for their effect upon separation performance using polyaromatic hydrocarbons (PAHs) and polar neutral pharmaceutical compounds. Attention is given to conditioning of the packed capillaries for high efficiency separations without necessity for sodium dodecyl sulfate (SDS). Separation conditions for the nonporous materials were modified from those previously determined on porous reversed-phase silica. Feasibility for method development and validation of a parent pharmaceutical compound and related impurities in the range of 0.1-120% of a 5 mg/mL concentration was assessed and reported. An approach to improving detection sensitivity through use of large-bore capillaries is briefly discussed.

Anthracenes↗
PubMed1998

Method development in pharmaceutical analysis employing capillary electrochromatography.

Capillary electrochromatography (CEC) has been employed to explore method development for a series of structurally related polar neutral compounds of pharmaceutical relevance. Capillaries with dimensions of 75 microm ID x 25 cm length (34.5 cm total) were packed with Spherisorb ODS-1, Hypersil phenyl, and Hypersil MOS (all 3 microm particles) and were compared in the reversed-phase mode in order to determine which phase provided the best initial performance and thus serve as the phase of choice for additional method development experiments. The various separation parameters examined for their effect on efficiency, k', resolution, and linear velocity included percent and type of organic modifier, buffer concentration, voltage, and temperature. All separations were conducted with an acidic mobile phase (aqueous mobile phase component, pH 3.0). The separation efficiencies obtained were on the order of 200,000-260,000 plates/m, which equates to reduced plate heights of 1.22 for columns packed with Spherisorb ODS-1. Repeatable column-to-column separation performance was demonstrated.

Acetonitriles↗
PubMed1997

Comparison of measures of visual acuity in infants: Teller acuity cards and sweep visual evoked potentials.

PURPOSE: This study compares the development of acuity in the same infants during one testing session using Teller acuity cards (TAC) and sweep visual evoked potentials (sVEP). We asked whether different testing methods in two centers would produce different developmental time courses. METHODS: Forty-eight infants were tested in two centers. The standard procedure for TAC was used. For sVEP acuity, the amplitude response curve derived from time-locked cortical activity was used to extrapolate to zero response, giving an acuity estimate for each infant. RESULTS: sVEP acuity was generally higher than TAC acuity. The rate of development was steeper for TAC than sVEP acuity with TAC starting at a much lower level. The ratio of sVEP to TAC acuity decreased exponentially with age reaching an asymptote of about 1.44 at 6 months. CONCLUSIONS: Results were indistinguishable between centers suggesting that comparison of acuity measures obtained using variations of these methods across centers is possible.

Aging↗
PubMed1991

Ion-pairing high-performance liquid chromatographic method for the determination of 5-aminosalicylic acid and related impurities in bulk chemical.

An ion-pairing high-performance liquid chromatographic method has been developed for the determination of 5-aminosalicylic acid (5-ASA) bulk chemical in the presence of thirteen potential synthetic process impurities. In addition, the method is suitable for the determination of the in process intermediate, 5-nitrosalicylic acid. A selective method was achieved on a Hypersil-BDS reversed-phase column using 1-heptanesulfonic acid sodium salt as the ion-pairing reagent in a 0.08 M sodium phosphate buffer (pH 2) containing 0.005 M 1-heptanesulfonic acid sodium salt and 0.07 M sodium chloride-methanol-tetrahydrofuran (85:11:4, v/v/v) isocratic mobile phase. The method was validated using a multi-day, intra-laboratory protocol. The validation addressed linearity, accuracy, precision, sensitivity, and ruggedness of the method. The validated method characterizes the purity of 5-ASA bulk chemical.

Aminosalicylic Acids↗
PubMed1991

Mechanism of misoprostol stabilization in hydroxypropyl methylcellulose.

The stability of misoprostol oil is significantly improved in a hydroxypropyl methylcellulose (HPMC) dispersion (1:100). In order to understand the enhanced stability of misoprostol oil in HPMC, the physical state of misoprostol oil in HPMC films was investigated using differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and transmission IR (TIR). Further, to determine the effect of polymer structure and the mobility of both water and misoprostol on misoprostol stability, the rate of misoprostol degradation was investigated in the misoprostol/HPMC dispersion (1:100) at 55 degrees C. The water sorption isotherm of the dispersion at 55 degrees C was determined, at seven different relative humidities, ranging from zero to 81%. The DSC and DMA measurements indicated that misoprostol oil, up to 29% in dry weight, is molecularly dispersed in the glassy HPMC. The TIR studies showed no evidence of complexation between misoprostol and HPMC. Stability studies of the misoprostol/HPMC (1:100) dispersion indicated that the first-order rate constants for misoprostol degradation increased in a concave-up fashion as the water content of the dispersion increased. Below two percent water content, the rate of misoprostol degradation was found to be minimal. Overall, it is suggested that misoprostol is stabilized in the dispersion by being molecularly dispersed in HPMC. Further, the glassy state of HPMC should reduce the mobility of misoprostol and water, leading to a minimal rate of degradation for misoprostol at low moisture levels.

Calorimetry, Differential Scanning↗
PubMed1990

Stabilization of misoprostol with hydroxypropyl methylcellulose (HPMC) against degradation by water.

The stability of misoprostol oil is significantly improved in a hydroxypropyl methylcellulose (HPMC) dispersion (1:100). In order to assess the effect of water on misoprostol stability, the rate of misoprostol degradation was investigated in the misoprostol/HPMC dispersion at 55 degrees C, along with the water sorption isotherm, under seven different relative humidity (RH) conditions ranging from 0 to 81%. The results indicated that the first-order rate constants of misoprostol degradation increased in a concave-up fashion as the water content of the dispersion increased. Below 30% relative humidity (approximately 2% water), the first-order rate constants of misoprostol degradation were found to be minimum. The results of the stability study were interpreted in terms of the changing structure of HPMC as it related to the mobility of water and misoprostol within the HPMC dispersion.

Adsorption↗
PubMedDate not supplied

Use of cerebellar cGMP in the measurement and characterization of the diazepam/ethanol interaction.

The characterization and measurement of the benzodiazepine and ethanol interaction has been of major interest for many years. Various pharmacological and biochemical studies have been employed to investigate this interaction, which is believed to occur predominantly in the CNS, but localization of one particular brain area has not been investigated. This research employed the rat cerebellum as a site to study the diazepam/ethanol interaction. The measurement of cerebellar ethanol and diazepam, by gas chromatography, demonstrated an enhancement of diazepam levels by ethanol. Ethanol and diazepam, alone and in combination, displayed a significant depression of cerebellar 3',5'-Guanosine Cyclic Monophosphate (cGMP). The depression seen by the combination was significantly greater than the simple algebraic sum, but insignificantly different from the corrected algebraic sum. The double reciprocal plot of the data demonstrated a common ordinate intercept for the diazepam line and the diazepam/ethanol (2 g/kg) line, thus indicating a competitive mechanism of action.

Animals↗