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S Furlanetto

Publications and source records attributed to S Furlanetto.

32 records · Page 2Linked to original sources
PubMed2000

Analysis of ACE-inhibitors by CE using alkylsulfonic additives.

Capillary electrophoresis (CE) was applied to the determination of angiotensin-converting enzyme (ACE) inhibitors in pharmaceuticals (tablets). Since a free solution CE system failed to reach a complete separation of closely related compounds (lisinopril, ramipril, benazepril, quinapril), alkylsulfonic additives (sodium heptansulfonate and (+)-10-camphorsulphonic acid) were added to the running buffer: improved separations were obtained suggesting a favourable effect of ion-pairing interactions between analytes and additives. The separations were carried out in acidic medium and a systematic investigation of electrophoretic parameters was made to evaluate the performance of the selected additives. Under the optimized conditions, ramipril and benazepril in their commercial dosage forms were determined confirming the applicability of the developed CE approach to the analysis of pharmaceutical samples; the results were also compared with those obtained applying a previously described and validated HPLC method.

Angiotensin-Converting Enzyme Inhibitors↗
PubMed2000

High-performance liquid chromatographic assay of erythromycin from biological matrix using electrochemical or ultraviolet detection.

Two chromatographic methods were developed for the determination of erythromycin A (EA) residues in animal tissues (muscle, liver, kidney and fat of cattle, pigs and poultry) and cow's milk. In addition to a more traditional method using electrochemical detection, we developed an original alternative method based on UV detection at 236 nm, by pretreating to create a chromophore in the molecule. An internal standard was used with both methods to check the variability of the analytical system. Analysis times and performance were compared. The recovery of EA from various matrices was greater than 95%. For both methods the quantification limit for EA was 0.25 microgram ml-1 for plasma, 0.025 microgram g-1 for milk and 0.125 microgram g-1 for the other biological matrices. The methods can be used to check for EA residues in these matrices; in fact, the statutory maximum residue limits (MRLs) of EA are 0.4 microgram g-1 in muscle, kidney, liver and fat of beef cattle, sheep, pigs and poultry, and 0.04 microgram g-1 in cow's and sheep's milk.

Adipose Tissue↗
PubMed1999

Influence of the preparation method on the physicochemical properties of ketoprofen-cyclodextrin binary systems.

Binary systems of ketoprofen with native crystalline beta-cyclodextrin and amorphous statistically substituted methyl-beta-cyclodextrin were investigated for both solid phase characterization (Differential Scanning Calorimetry, powder X-ray diffraction, Infrared Spectroscopy, Scanning Electron Microscopy) and dissolution properties (dispersed amount and rotating disc methods). Grinding, kneading, sealed-heating and colyophilization of equimolar combinations of ketoprofen with methyl-beta-cyclodextrin, as well as colyophilization of analogous combinations with beta-cyclodextrin, led to amorphous products. Crystalline drug, instead, was still clearly detectable in coground, kneaded and sealed-heated products with beta-cyclodextrin. Both the preparation method, and even more the nature of the carrier, played an important role in the performance of the system. Colyophilized and sealed-heated products showed the best dissolution properties. However, independently of the preparation technique, all combinations with methyl-beta-cyclodextrin yield better performances than the corresponding ones with the beta-cyclodextrin. Moreover, intrinsic dissolution rate of ketoprofen from simple physical mixture with the beta-cyclodextrin derivative was even five-fold higher than that from the best product with the parent beta-cyclodextrin.

Anti-Inflammatory Agents, Non-Steroidal↗
PubMed1998

Development and validation of a differential pulse polarographic method for quinolinic acid determination in human plasma and urine after solid-phase extraction: a chemometric approach.

A chemometric approach was applied for determining quinolinic acid in human plasma by differential pulse polarography after solid phase extraction. A fractional factorial design was used to examine the significant experimental variables for the peak height maximization. A Doehlert design, which allowed a sequential response surface methodology to be performed, was applied to the variables scan rate and drop size. The results indicated that the scan rate had the greatest effect on the response peak height. The linear range was extended from 8.52 x 10(-8) to 1.34 x 10(-5) M and the limit of detection was 2.9 x 10(-8) M. The validation process consisted of a pre-validation study followed by the main validation in the plasma matrix. The robustness and the intermediate precision were evaluated by means of experimental design. A 3(4)//9 screening symmetric matrix and a central composite design were used to optimize the solid phase extraction procedure of the analyte from human plasma using anion exchange cartridges. The goal was to select the best retention, wash and elution solvents and their volumes in order to maximize the extraction efficiency using as the response the polarographic peak height. An extraction efficiency of 90% was found. The method was also applied to the determination of quinolinic acid in urine and the mean concentration in human plasma and urine, was found to be 3.7 x 10(-7) and 4.9 x 10(-5) M respectively.

Chemistry Techniques, Analytical↗
PubMed1998

Set-up and validation of an adsorptive stripping voltammetric method for kynurenic acid determination in human urine.

Validation of an adsorptive stripping voltammetric method for kynurenic acid determination in urine, was presented. The selection of appropriate validation parameters, the design consideration for evaluation and the problem of endogenous metabolites were discussed. The considered fundamental criteria for assessing the reliability and overall performance of the method in the urine matrix were selectivity, linearity and range, limit of quantitation, accuracy, precision and analyte stability. The intermediate precision was also evaluated by means of a full factorial design. An HPLC method with fluorimetric detection was used as a reference method to assess the accuracy. The analysis in urine required a pH control as pointed out by robustness testing and the found kynurenic acid concentration in daily urine ranged from 5 to 40 microM.

Adsorption↗
PubMed1998

Thermal analysis as a screening technique in preformulation studies of picotamide solid dosage forms.

The potential compatibilities of several commonly used pharmaceutical excipients with picotamide were evaluated using differential scanning calorimetry (DSC). The effects of aging and of mechanical treatment (blending, grinding, or kneading) of samples were also evaluated. Hot-stage microscopy (HSM) and scanning electron microscopy (SEM) were used as complementary techniques to implement and assist in interpretation of the DSC results. DSC analysis evidenced a noticeable modification of drug thermal features in the mixtures with palmitic acid, stearic acid, stearyl alcohol, polyethylene glycol (PEG) 20,000, and sorbitol, but HSM analysis showed that the DSC behavior was mainly because of the drug dissolution in the melted excipient, which allowed the presence of important solid-solid interactions to be excluded. Compatibility with Mg stearate was also found, even if sample manipulation induced the partial conversion of Mg stearate in a pseudo-polymorphic modification. Mechanical stress displayed an increased hygroscopicity of mixtures with glucose and lactose, as well as some solid-solid interactions with lactose and mannitol.

Calorimetry, Differential Scanning↗
PubMed1997

Experimental design strategies in the optimization and robustness testing of adsorptive stripping voltammetric conditions for kynurenic acid determination.

Experimental design was used for the optimization and robustness testing of an adsorptive stripping voltammetric procedure for kynurenic acid determination. The optimization of the peak height response proceeded through a screening phase (D-optimal design strategy) followed by a response surface study (Doehlert design) applied to the variables pH, pulse amplitude and stirring rate. An interaction between pH and stirring rate was pointed out. The optimized method was validated and the variation of factors that was expected to occur in practice was simulated in a robustness test. A composite fractional matrix for the evaluation of method robustness was used and pH emerged as the only critical factor. The linear range found applying the optimized conditions was 2.5 x 10(-9) to 2.5 x 10(-7) M and the calculated limit of detection was 1.72 x 10(-9) M.

Adsorption↗
PubMed1996

Experimental design in the development of voltammetric method for the assay of omeprazole.

A multivariate strategy was used to optimize an adsorptive stripping voltammetric method for the determination of the antiulcer drug omeprazole. A 3/4 matrix was used for the variable screening while a central composite design was chosen in the subsequent step to evaluate the response surfaces. Simultaneous optimization of the response peak height (hp) and peak half width w1/2), the latter being a peak shape measure, was achieved. The factors accumulation time, pulse amplitude, scan rate and stirring rate were all found to be statistically significant for the response hp, while for the response w1/2 only the stirring rate was found to be significant. The optimized method shows a good linearity between peak height and analyte concentration in the concentration range from 8.33 x 10(-9) M to 1.42 x 10(-7) M with a LOD of 6.5 x 10(-9) M. The mean recovery of omeprazole in capsules was 101.9% with a SD of 2.04 (RSD = 200).

Adsorption↗
PubMed1995

Design and optimization of the variables in the adsorptive stripping voltammetric determination of rufloxacin in tablets, human plasma and urine.

An adsorptive stripping voltammetric method with a hanging mercury drop electrode was developed for the determination of the fluoroquinolone rufloxacin in tablets, human plasma and urine. Measurements were obtained in differential pulse mode and a multivariate strategy was used to optimize the variables involved. Besides the independent effects of the variables, a strong interaction between scan rate and pulse duration has been found. Rufloxacin was analysed at concentrations between 1.7 x 10(-8) and 1.9 x 10(-7) M with a detection limit of 9.2 x 10(-9) M. Diluted tablet solutions and urine samples were analysed directly, while plasma samples needed an extraction procedure before voltammetric analysis. An improved HPLC procedure was used as comparative method.

Absorption↗
PubMed1994

High-performance liquid chromatographic determination of benzalkonium and naphazoline or tetrahydrozoline in nasal and ophthalmic solutions.

A high-performance liquid chromatographic method is described for the determination of benzalkonium chloride homologues and naphazoline nitrate or tetrahydrozoline hydrochloride in ophthalmic and nasal solutions. The technique involves a one-step dilution (1:5) for sample preparation and direct injection onto a 5 mm RP C-8 column. The mobile phase is acetonitrile-diluted acetic acid (80:20, v/v) with 6 mM tetramethylammonium bromide. Detection is carried out at 260 nm with a diode array. The method is rapid, specific, reproducible and is especially useful for quality control procedures.

Benzalkonium Compounds↗
PubMedDate not supplied

Planar chromatographic and liquid chromatographic analysis of thiamphenicol in bovine and human plasma.

A planar chromatographic (PC) method was developed to determine thiamphenicol in human and bovine plasma with florphenicol as internal standard. The performance of the method was compared with that of a liquid chromatographic method. Recovery of extraction method developed for plasma was 81.51 +/- 2.85%. Reproducibilities of the PC assay performed with various PC plates were also good.

Animals↗