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showing 10 items of 782 documents
Simultaneous determination of acetylsalicylic acid and caffeine in pharmaceuticals by flow injection with fourier transform infrared detection.
1993
Abstract A fast quality control methodology has been developed for the simultaneous determination of acetylsalicylic acid (ASA) and caffeine in pharmaceuticals by flow injection—Fourier Transform Infrared Spectrometry. The method is based on the solubilization of ASA and caffeine in CH2Cl2 and the use of a flow system to introduce samples and standards in the spectrometer. Two solutions, containing 90 and 110% of the reported concentration of the two active principles in the sample, were employed in order to control the extreme tolerance levels accepted by the International Pharmacopeia for the composition of formulations. A 300 μl volume of each solution was injected in turn, into a carrie…
The solubilization site of 5,10,15,20-tetrakis-(2,6-dichlorophenyl)-porphyrin-Mn(III) in DPPC vesicles: A spectrophotometric and tensiometric study
2006
Abstract The solubilization site of 5,10,15,20-tetrakis-(2,6-dichlorophenyl)-porphyrin-Mn(III) (MnTDPPC) in l -α-dipalmitoylphosphatidyl choline (DPPC) vesicles was determined in a systematic UV–vis spectrophotometric study. Measurements of the MnTDPPC absorbance have been conducted at constant temperatures (in the interval 30 °C ≤ T ≤ 48 °C) and varying concentrations of phospholipid. In the entire temperature range, the absorption due to MnTDCCP was found to increase with increasing DPPC concentration, until it reaches a plateau value. The data have been analyzed using a pseudo-phase model yielding the binding constant of MnTDCPP to vesicular aggregates. No significant temperature depende…
Filter-based infrared detectors for high temperature size exclusion chromatography analysis of polyolefins: calibration with a small number of standa…
2012
Infrared detection has been shown to be very appropriate for high temperature analysis of polyolefins. After some early reports in which dispersive or single-band filter-based detectors were applied, Fourier transform detectors have been described for this application, in order to improve the method sensitivity. Modern simple filter-based detectors prove, however, comparable sensitivity while providing a number of practical advantages when coupled to chromatographic systems: reduced cell volume, simplified hardware, continuous generation of absorbance chromatograms, as well as simpler data collection and processing. A practical method for calibration, using multiple-band signals obtained wi…
Kinetic-Spectrophotometric Determination of Primary and Secondary Amines by Reaction with 1-2 Naphthoquinone-4-Sulphonate.
1994
Abstract A kinetic-spectrophotometric method for the determination of primary and secondary amines is described. It is based on the coloured reaction of these amines with sodium 1,2 Naphthoquinone 4-sulphonate (NQS) in the presence of a non-ionic surfactant. For each determination the optimum conditions were studied and found to be as follows: pH 10.5. Carbonate-bicarbonate buffer 0.1M, Triton X-100 0.1%, Temperature 45°C, and NQS 6.4 × 10−3 M and interval of time 45–180s at wavelength 490 nm. The parameters used for the quantitative determinations are the reaction rate and the increase in the absorbance of the kinetic curves. This procedure has been applied to the determination of ephedrin…
A comparison of various calibration techniques applied to the ninhydrin-cefoxitin determination
1996
Abstract This report deals with spectrophotometric determination of cefoxitin from intact antibiotics or from its acid induced degradation product by means of their reaction with ninhydrin in a strong sulphuric acid medium. To obtain the calibration graphs four methods were used: absorbance of reacted cefoxitin against a reagent blank as an analytical signal, first-derivative signal of absorbance against a water blank as an analytical signal, first-derivative signal of absorbance against a reagent blank as an analytical signal and the H-Point Standard Additions Method (HPSAM) by using absorbance increment values as analytical signals. The HPSAM is applied to the determination of cefoxitin i…
Optical studies on the specific interaction of dipyridamole with alpha 1-acid glycoprotein (orosomucoid).
1982
Abstract The interaction of dipyridamole with α1-acid glycoprotein was investigated by circular dichroism and ultraviolet absorbance measurements as well as by equilibrium dialysis experiments. Dipyridamole is bound to the protein via one site of extremely high affinity and by at least one site of considerably lower affinity. Only the association of dipyridamole with the high affinity site produces typical extrinsic Cotton effects. As a result of experimental observations it is concluded that the high affinity site is located in a hydrophobic protein structure of the glycoprotein.
Development and validation of a micellar liquid chromatographic method to determine three antitumorals in plasma
2017
Aim: A micellar liquid chromatographic method to determine several anticancer drugs (pazopanib, dabrafenib and regorafenib) in plasma was developed and validated by the guidelines of the EMA. Experimental: Plasma samples were directly injected, after a 1/5-dilution in a micellar solution. The drugs were resolved in <18 min using a C18 column. The mobile phase was an aqueous solution of 0.12 M SDS – 2% 1-pentanol, buffered at pH 7. The detection was performed by absorbance at 260 nm. Results: The values of the main validation parameters were: LOD (0.1–1 mg/l), calibration range (0.2–2 to 80 mg/l), accuracy (-12.5 to +11.7%) and precision (<11.9%). Conclusion: The procedure was conduct…
Comparison of several methods used for the determination of cephalosporins. Analysis of cephalexin in pharmaceutical samples
2002
The precision of UV absorbance of intact and acid degraded cephalosporins, ninhydrin, high performance liquid chromatography and iodometric methods used for analysis of cefoxitin, cefotaxime, cephazolin and cephalexin were compared. To obtain the calibration graphs the analytical signal used were: absorbance, first derivative absorbance, second derivative absorbance and H-point Standard Additions Method by using absorbance values at two selected wavelengths as analytical signal. These methods and calibration graphs were also used for the determination of cephalexin in pharmaceutical samples.
In situ generation of Co(II) by use of a solid-phase reactor in an FIA assembly for the spectrophotometric determination of penicillamine
2005
[EN] A flow injection analysis (FIA) manifold for the determination of penicillamine in pharmaceutical preparations is proposed. The manifold includes a solid-phase reactor for the in situ production of the derivatizing reagent, Co(II) ion, which forms a coloured complex with penicillamine in an alkaline medium. The reactor is prepared by natural immobilization of cobalt carbonate on a polymer matrix, which endows it with a high mechanical and microbiological stability. The cobalt released by passage of a 5 x 10(-4) Mol l(-1) sulphuric acid stream at a flow-rate of 2.3 ml min(-1) is merged with a volume of 314 mu l of sample containing penicillamine in ammonium-ammonia buffer at pH 9.5 to m…
Self‐esteem mediates the associations among negative affect, body disturbances, and interpersonal problems in treatment‐seeking obese individuals
2015
Background: This study investigated the relationship among negative affect, body image disturbances (BID), and interpersonal problems, and the mediat- ing effect of self-esteem in a group of treatment-seeking obese individuals. Methods: Four hundred twenty-two obese patients (85 males and 337 females) completed standardised measures that assessed negative affect, BID, self-esteem, and interpersonal problems. Results: Structural equation modelling showed that obese individuals with greater negative affect and BID reported higher interpersonal problems and that self-esteem mediated the relationships among negative affect, BID, and interpersonal problems. Conclusions: The mediating role of sel…