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At least 253 records · Page 14Linked to original sources
PubMed2005

Application of first-derivative, ratio derivative spectrophotometry, TLC-densitometry and spectrofluorimetry for the simultaneous determination of telmisartan and hydrochlorothiazide in pharmaceutical dosage forms and plasma.

Four sensitive methods are described for the direct determination of telmisartan (TELM) and hydrochlorothiazide (HCT) in combined dosage forms without prior separation. The first method is a first derivative spectophotometry (1D) using a zero- crossing technique of measurement at 241.6 and 227.6 nm for TELM and HCT, respectively. The second method is the first derivative of ratio spectrophotometry (1DD) where the amplitudes were measured at 242.7 nm for TELM and 274.9 nm for HCT. The third method is based on TLC separation of the two drugs followed by the densitometric measurements of their spots at 295 and 225 nm for TELM and HCT, respectively. The separation was carried out on silica gel 60 F254 using butanol: ammonia 25% (8:2 v/v) as mobile phase. The fourth method is spectrofluorimetric determination of TELM, depending on measuring the native fluorescence of the drug in 1 M sodium hydroxide at lambda excitation 230 nm and emission at 365 nm. The proposed methods were applied successfully for the determination of the two drugs in bulk powder and in pharmaceutical formulations. The spectrofluorimetric method was utilized for the analysis of TELM in human plasma.

Benzimidazoles↗
PubMed2004

Reflectance spectrophotometry for the assessment of mucosal perfusion in the gastrointestinal tract.

Reflectance spectrophotometry (RS) is an optical technology that has been used for nearly three decades in the measurement of tissue hemoglobin oxygen saturation in the gastrointestinal tract. The technology has evolved substantially throughout this period,and commercial devices are now available for use in clinical trials. Numerous studies have used RS to investigate the importance of mucosal perfusion in disorders such as ulcer disease, portal hypertension, and septic shock. More recently, the technique has been applied to measure changes in perfusion in response to infusion of vasoactive medications and maneuvers such as cardiopulmonary bypass. The results of current trials investigating the application of RS in critical care monitoring and vascular interventions will likely determine whether the technique will evolve from predominantly a research tool to a clinically useful device.

Gastric Mucosa↗
PubMed2004

Determination of lisinopril in dosage forms and spiked human plasma through derivatization with 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) followed by spectrophotometry or HPLC with fluorimetric detection.

Two sensitive, simple and specific methods based on spectrophotometry and reversed-phase HPLC with fluorimetric detection are described for the determination of lisinopril in dosage forms as well as in spiked human plasma using solid phase extraction (SPE) procedures. Both methods are based on the derivatization of lisinopril with 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in borate buffer of pH 9 to yield a yellow, fluorescent product. The spectrophotometric method depends on measuring the formed yellow color at 470 nm after optimization of the reaction conditions. The HPLC method is based on measurement of the derivatized product using fluorescence detection at 540 nm (excitation at 470 nm). The separation of the derivatized drug, the excess reagent and the internal standard (bumetanide) was performed on a reversed-phase ODS column using isocratic elution with methanol-0.02 M sodium dihydrogen phosphate, pH 3.0 (55:45, v/v) at a flow rate of 1.0 ml/min. The calibration graphs were linear over the concentration ranges 2-20 or 0.02-3.2 microg/ml of lisinopril with minimum detectability of 0.3 and 0.008 microg/ml (6.1 x 10(-7) and 1.7 x 10(-8)M) for the spectrophotometric and the HPLC methods, respectively. The proposed methods were applied without any interference from the tablet excipients for the determination of lisinopril in dosage forms, either alone or co-formulated with hydrochlorothiazide. Furthermore, the use of the HPLC method was extended to the in vitro determination of the drug in spiked human plasma. Interference from endogenous amino acids has been overcomed by using the solid phase extraction technique, the percentage recovery (n=6) was 101.6+/-3.35.

4-Chloro-7-nitrobenzofurazan↗
PubMed2004

Using spectrophotometry to determine in vitro turnover rates of peptides in plasma.

A new method for determination of first-order elimination constants for dipeptides is presented. The peptides are hydrolysed by plasma enzymes into amino acids, and ortho-phthaldialdehyde (OPA) is used to react with free primary amino groups. The concentration of free amino groups can, thus, be followed using simple spectrophotometry. A mathematical model for the concentration of free primary amino groups with time is presented through which the elimination constant, and thus the half life, can be determined by curve fitting. The method is applied to inhibitors of angiotensin-converting enzyme derived from the primary structure of milk proteins. The results show that these dipeptides have in vitro half lives ranging from 4.3-64 min, when incubated with 50% rat plasma. This explains why these casokinins in vivo only cause a very moderate and short-lasting inhibition. The model for calculation of elimination constant is limited to dipeptides that do not contain a C-terminal proline. The derivatization method can be applied to longer peptides as a crude indicator of peptide hydrolysis, but does not allow calculation of their elimination constants per se.

Animals↗
PubMed2006

Determination of Co(II) in water and soil samples using spectrophotometry coupled with preconcentration on 4-amino methyl pyridine anchored silica gel column.

4-amino methyl pyridine anchored silica gel (4-AMPS) was used as a sorbent in a simple sensitive spectrophotometry determination of Co(II) in various samples using piperazine dithiocarbamate as a color developing agent (lambda(max)=390 nm) at pH 5.0+/-0.2. Beer's law was obeyed over the range of 0.1-5.0 microg ml(-1). The molar absorptivity and Sandell's sensitivity were 1.257x10(5) lmol(-1) cm(-1) and 0.006145 microg cm(-2), respectively. Under these conditions, the preconcentration factor obtained was 80, and the detection limit achieved was 5.0 ng ml(-1). The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Co(II) from various samples range from 97.50 to 99.66%. The present method was successfully applied for the determination of Co(II) in various water and soil samples. The proposed method was compared with reported methods in terms of Student's 't'-test and variance ratio 'f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

Adsorption↗
PubMed2006

A critical study on the application of the zero-crossing derivative spectrophotometry to the photodegradation monitoring of lacidipine.

An extensive study on the application of the "zero-crossing" technique for the analysis of a binary mixture of the photosensitive drug lacidipine and its corresponding by-product by derivative spectrophotometry is described. The technique has been compared to either conventional and recently developed UV spectrophotometric procedures, including chemometric methods. The prediction ability of the different analytical techniques has been checked by using the first-order derivative spectra of drug and photoproduct in binary mixtures. Relative advantages and drawbacks have been discussed. The zero-crossing technique suffers from several limitations, mostly ascribed to the selection of suitable signals along slopes of the spectral curve, giving rise to low accurate and precise results. The mean recovery from the zero-crossing analysis was calculated to lie in the 95.1-98.4% range for lacidipine, and 91.2-118.9% for the photoproduct. Chemometric methods showed a greater prediction ability with a 101.4-103.0% and 96.3-98.4% recovery for drug and degradation product, respectively.

Dihydropyridines↗
PubMed2006

Simultaneous determination of lamivudine and stavudine in antiretroviral fixed dose combinations by first derivative spectrophotometry and high performance liquid chromatography.

Two methods are described for the simultaneous determination of lamivudine (3TC) and stavudine (d4T) in combined pharmaceutical tablets. The first method depends on first derivative UV-spectrophotometry with zero-crossing measurement technique. The first derivative absorbances at 280 and 300 nm were selected for the determination of stavudine and lamivudine, respectively. The second method is based on the separation of both drugs by high performance liquid chromatography using methanol:water (20:80) as the mobile phase at 0.6 ml/min on a reverse phase column with detection at 270 nm. Both the methods showed good linearity, reproducibility and precision. No spectral or chromatographic interferences from the tablet excipients were found. The proposed methods were suitably applied to the assay of commercial formulations. The procedures were rapid, simple and suitable for routine quality control application.

Chromatography, High Pressure Liquid↗
PubMed2005

Quantitative spectrophotometry using integrating cavities.

Absorption spectrophotometry, a standard tool for quantitative analysis, suffers from two major drawbacks: lack of sensitivity and vulnerability to scattering. It has been pointed out earlier that the solution to these problems lies in using a reflecting cavity as a sample holder. Due to multiple reflections at the cavity wall, the effective pathlength becomes considerably larger than the diameter of the cavity, and scattering losses are eliminated because scattered light is prevented from escaping the detector. Though much effort has been spent in analysing and improving the performance of such a device, often called an integrating cavity absorption meter (ICAM), a simple strategy for deducing the absorbance of the sample is still lacking. It is shown here that the absorbance A' measured by using an ICAM exhibits a sublinear increase with the solute concentration C. The physical reason for this departure from linearity is explained, and a straightforward procedure for converting A' to the true absorbance A (proportional to C) is established. The reliability of the procedure is demonstrated by comparing the ICAM absorption spectrum of dilute dye solutions with the spectra of more concentrated solutions recorded in a conventional spectrophotometer. The ability of the device to cope with scattering was tested by filling the ICAM with a suspension of chloroplasts, and the spectrum was found, as expected, to be free from scattering artefacts.

Calibration↗
PubMed2005

Evaluation of the acidity constants of the 4-hidroxy-5-[salicylideneamino]-2-7-naphthalenedisulfonic acid (Azomethine-H) using UV-vis spectrophotometry.

The time stability of the azomethine-H species was determined not to be better than 10 min in the absence of oxygen and light, however under phosphate buffered conditions the azomethine-H species remained stable for longer periods, as indicated by the spectrophotometric behaviour. Nevertheless, the analysis time still exceeded the stability allowance. Therefore, the determination of the acidity constants of the Azomethine-H species was studied by means of UV-vis spectrophotometry in buffered media by means of the point-by-point analysis and data processing with SQUAD to refine the resulting constants, which were: pK(a1) = 3.39, pK(a2) 7.36 and pK(a3) 8.73. The latter were associated to the corresponding acid-base equilibria of the amine and hydroxy groups constituting the molecule.

Buffers↗
PubMed2005

Determination of myoglobin based on its enzymatic activity by stopped-flow spectrophotometry.

A new method has been developed for the determination of myoglobin (Mb) based on its enzymatic activity for the oxidation of o-phenylenediamine (OPDA) with hydrogen peroxide. Stopped-flow spectrophotometry was used to study the kinetic behavior of the oxidation reaction. The catalytic activity of Mb was compared to other three kinds of catalyst. The time dependent absorbance of the reaction product, 2,3-diamimophenazine (DAPN), at a wavelength of 426 nm was recorded. The initial reaction rate obtained at 40 degrees C was found to be proportional to the concentration of Mb in the range of 1.0 x 10(-6) to 4.0 x 10(-9)mol L(-1). The detection limit of Mb was found to be 9.93 x 10(-10)mol L(-1). The relative standard deviations were within 5% for the determination of different concentrations of Mb. Excess of bovine serum albumin (BSA), Ca(II), Mg(II), Cu(II), glucose, caffeine, lactose and uric acid did not interfere.

Animals↗
PubMed2006

H-point standard addition method--first derivative spectrophotometry for simultaneous determination of palladium and cobalt.

H-point standard addition method (HPSAM) has been applied for simultaneous determination of palladium and cobalt in trace levels, using disodium 1-nitroso-2-naphthol-3, 6-disulphonate (nitroso-R salt) as a selective chromogenic reagent. Palladium and cobalt in the neutral pHs form red color complexes with nitroso-R in aqueous solutions and making spectrophotometric monitoring possible. Simultaneous determination of palladium and cobalt were performed by HPSAM--first derivative spectrophotometry. First derivative signals at the two pairs of wavelengths, 523 and 589 nm or 513 and 554 nm were monitored with the addition of standard solutions of palladium or cobalt, respectively. The method is able to accurately determine palladium/cobalt ratio 1:10 to 15:1 (wt/wt). Accuracy and reproducibility of the determination method on the various amounts of palladium and cobalt known were evaluated in their binary mixtures. To investigate selectivity of the method and to ensure that no serious interferences were observed the effects of diverse ions on the determination of palladium and cobalt were also studied. The recommended procedure was successfully applied to real and synthetic cobalt or palladium alloys, B-complex ampoules, a palladium-charcoal mixture and real water matrices.

Alloys↗
PubMed2005

Studies on the oxidation reaction of tyrosine (Tyr) with H2O2 catalyzed by horseradish peroxidase (HRP) in alcohol-water medium by spectrofluorimetry and differential spectrophotometry.

An oxidation reaction of tyrosine (Tyr) with H(2)O(2) catalyzed by horseradish peroxidase (HRP) was studied by spectrofluorimetry and differential spectrophotometry in the alcohol(methanol, ethanol, 1-propanol and isopropanol)-water mutual solubility system. Compared with the enzymatic-catalyzed reaction in the water medium, the fluorescence intensities of the product weakened, even extinguished. Because the addition of alcohols made the conformation of HRP change, the catalytic reaction shifted to the side of polymerization and the polymer (A(n)H(2), n>or=3) exhibited no fluorescence. The four alcohols cannot deactivate HRP. Moreover isopropanol activated HRP remarkably.

Alcohols↗
PubMed2005

Simultaneous determination of titanium and molybdenum in steel samples using derivative spectrophotometry in neutral micellar medium.

A simple, selective and sensitive spectrophotometric method has been developed for the individual and simultaneous determination of Ti(IV) and Mo(VI) using resacetophenone p-hydroxybenzoylhydrazone (RAPHBH) in presence of Triton X-100, without any prior separation. Beer's law is obeyed between 0.13-1.2 microg mL-1 and 0.18-1.90 microg mL-1 concentration of Ti(IV) and Mo(VI) at 455 nm and 405 nm, respectively. The molar absorptivity and Sandell's sensitivity of the coloured complexes at pH 3.0 are 3.1x10(4) L mol-1 cm-1, 4.2x10(4) L mol-1 cm-1, and 1.6 ng cm-2, 2.3 ng cm-2 for Ti(IV) and Mo(VI), respectively. The stoichiometry of the complexes were found to be 1:2 and 1:1 (metal:ligand) for Ti(IV) and Mo(VI), respectively. These metal ions interfere with the determination of each other in zero-order spectrophotometry. The first derivative spectra of these complexes permitted a simultaneous determination of Ti(IV) and Mo(VI) at zero crossing wavelengths of 500.0 nm and 455.0 nm, respectively. The effect of foreign ions in the determination of Ti(IV) and Mo(VI) were investigated. The proposed method has been successfully applied for the determination of titanium and molybdenum in standard alloy steel, mineral and soil samples.

Acetophenones↗
PubMed2006

Determination of the complexation constants of Pb(II) and Cd(II) with thymol blue using spectrophotometry, SQUAD and the HSAB principle.

This paper presents the results concerning the determination of the formation constants of the complexes between thymol blue, TB, and the metal ions Pb(II) or Cd(II). The experimental procedure was carried out in the presence of a nitrogen atmosphere at 25 degrees C. The spectrophotometry data obtained were processed through the software SQUAD to calculate the complexation constants of the metal-indicator and to establish an adequate base of the models which considered the structure of the indicator, and the actual metal species in the aqueous solutions. For the Pb(II)-TB-H2O system the logK value calculated for the PbTB complex was 5.591+/-0.057 while for the Cd(II)-TB-H2O system, the logK value of the CdTB complex was 5.099+/-0.008. Also, supporting theoretical chemistry results on the chemical hardness of TB molecule were performed to enable establishment of a relative prediction scale of the TB complexation constants ranking in the framework of the Principle of Hard and Soft Acids and Bases or HSAB Principle.

Cadmium Compounds↗
PubMed1970

Study of biological pigments by single specimen derivative spectrophotometry.

The single specimen derivative (SSD) method provides an absolute absorption spectrum of a substance in the absence of a suitable reference. Both a reference and a measuring monochromatic beam pass through a single sample, and the specimen itself acts as its own reference. The two monochromatic beams maintain a fixed wavelength difference upon scanning, and the difference in absorbance of the two beams is determined. Thus, the resulting spectrum represents the first derivative of the conventional type absorption spectrum. Tissues and cell fractions have been examined at room and liquid N(2) temperature and chromophoric molecules such as the mitochondrial cytochromes and blood pigments have been detectable in low concentrations. In the case of isolated cellular components, the observed effects of substrates and inhibitors confirm similar studies by conventional spectrophotometry. The extension of the SSD concept to the microscopic level has permitted the study of the tissue compartmentalization and function of cytochromes and other pigments within layered tissue.

Animals↗
PubMed2003

Kinetic study of alkaline induced hydrolysis of the skeletal muscle relaxant chlorzoxazone using ratio spectra first derivative spectrophotometry.

2-Amino-4-chlorophenol was found to be the alkaline induced degradation product and the synthetic precursor of chlorzoxazone. The aim of this work is to study different factors affecting the degradation process due to the high toxicity of 2-amino-4-chlorophenol. Chlorzoxazone was found to follow pseudofirst order kinetics. Ratio spectra first derivative spectrophotometry (DR(1)) was developed for monitoring the change in chlorzoxazone concentration during the degradation process. Kinetic parameters (rate constant (K) and half-life (t(0.5))) were calculated at different temperatures (40-120 degrees C) and different sodium hydroxide concentrations (3-10 M). Activation energy at 3 and 8 M sodium hydroxide concentration and alkaline induced catalysis constant at 60, 70 and 80 degrees C were also calculated.

Chlorophenols↗
PubMed1999

UVA/UVB sunscreen determination by second-order derivative ultraviolet spectrophotometry.

UVA/UVB protective agents are important constituents in many cosmetics and sunscreen preparations. Analytical methodologies which enable the determination of combined substances with different spectrophotometric characteristics are therefore useful and cost-effective. To this end, the following substances in a sunscreen gel were analyzed: the UVB and UVA protective substances, 2-hydroxy-4-methoxy-benzophenone-5-sulphonic acid (BZP) and 2-phenylbenzymidazole-5-sulphonic acid (PBS), respectively, were evaluated by second-order derivative ultraviolet spectrophotometry in distinct solvents and wavelengths. The method used for determination of BZP in 95% ethanol was the zero-peak (ZP) at 356.0 nm. For PBS, the solvent used was 0.1 mol l-1 triethanolamine, and the methods were the ZP at 317.5 nm and the peak-peak (PP) at 317.5-323.0 nm. Statistical results for the methods showed linearity of 0.9999 and an average precision of 1.12% (ZP) for BZP, and 0.55% (ZP) and 0.63% (PP) for PBS. The average recovery for BZP and PBS were 97.28% (ZP), 103.13% (ZP) and 103.71% (PP), respectively.

Benzimidazoles↗
PubMedDate not supplied

Octreotide decreases canine gastric mucosal blood flow: a controlled assessment by endoscopic reflectance spectrophotometry.

The aim of this study was to evaluate the effects of octreotide, a long-acting somatostatin analogue, on canine gastric mucosal blood flow and hemodynamics. We hypothesized that octreotide might decrease gastric mucosal blood flow without causing adverse hemodynamic effects. Two groups of dogs were anesthetized (six normal dogs and six dogs with prehepatic portal hypertension), and each dog was administered intravenous octreotide, normal saline solution, and vasopressin for 30 minutes on separate days in a blinded, randomized fashion. Vasopressin was included as treatment for a positive control. Gastric mucosal blood flow was assessed at the fundus, corpus, and antrum by endoscopic reflectance spectrophotometry. A femoral arterial catheter monitored systemic blood pressure and heart rate. Treatment responses for all observations were calculated for each dog as a percentage of baseline values. For mucosal blood flow, treatment responses did not differ significantly over time or between animal group or gastric location. Octreotide significantly decreased indices of hemoglobin concentration (-19%, p = 0.01) and oxygen saturation (-17%, p = 0.0002) compared to saline (-9% and -7%, respectively). The mean arterial pressure was increased after octreotide compared to saline (+23% versus +7%, p = 0.01), but octrotide had no effect on heart rate (+2% versus +1%). Vasopressin also decreased the indices of hemoglobin concentration (-34%) and oxygen saturation (-82%) significantly more than saline (p = 0.001). Vasopressin increased mean arterial pressure (+55%), but also caused reflex bradycardia (-22%) significantly more than saline (p = 0.001). We conclude that octreotide decreases canine gastric mucosal blood flow and appears to cause minimal hemodynamic changes.

Animals↗