[Ultraviolet spectrophotometric determination of tenoxicam using iodine solution as reagent].

PubMed

Mândrescu, Mariana; Spac, A F; Dorneanu, V

2009-01-01

For the tenoxicam determination (Nonsteroidal Antiinflammatory Drug - NSAID) it was developed a spectrophotometric method, after the coupling reaction of tenoxicam with iodine, in methanolic medium, with maximum of absorbance at 289 nm. The practical working conditions were established. In the 0.5 divided by 5.0 microg/mL range of tenoxicam concentration, were used 5 x 10(-3) M iodine solution and 0.5 N hydrocloric acid. The stability of product were evaluated for 30 minutes. The developed method was validated. The method showed a good linearity in the range of 0.5 divided 5.0 microg/mL (the correlation coefficient r = 0.9995). The detection limit (LD) was 0.14 microg/mL and the quantification limit (LQ) was 0.49 microg/mL. There were established the precison (RSD = 1.90%) and the accuracy-recovery in the range 97.27 divided by 102.56% with a mean recovery of 99.49%. The experimental results demonstrated a good sensibility. The specific absorptivity for this method is A1%(1 cm,289 nm) = 1770 much higher than tenoxicam in methanol (A1%(1 cm,360 nm) = 323).

Two spectrophotometric methods for simultaneous determination of some antihyperlipidemic drugs

PubMed Central

Abdelwahab, Nada S.; El-Zeiny, Badr A.; Tohamy, Salwa I.

2012-01-01

Two simple, accurate, precise and economic spectrophotometric methods have been developed for simultaneous determination of Atorvastatin calcium (ATR) and Ezetimibe (EZ) in their bulk powder and pharmaceutical dosage form. Method (I) is based on dual wavelength analysis while method (II) is the mean centering of ratio spectra spectrophotometric (MCR) method. In method (I), two wavelengths were selected for each drug in such a way that the difference in absorbance was zero for the second drug. At wavelengths 226.6 and 244 nm EZ had equal absorbance values; therefore, these two wavelengths have been used to determine ATR; on a similar basis 228.6 and 262.8 nm were selected to determine EZ in their binary mixtures. In method II, the absorption spectra of both ATR and EZ with different concentrations were recorded over the range 200–350, divided by the spectrum of suitable divisor of both ATR and EZ and then the obtained ratio spectra were mean centered. The concentrations of active components were then determined from the calibration graphs obtained by measuring the amplitudes at 215–260 nm (peak to peak) for both ATR and EZ. Accuracy and precision of the developed methods have been tested; in addition recovery studies have been carried out in order to confirm their accuracy. On the other hand, selectivities of the methods were tested by application for determination of different synthetic mixtures containing different ratios of the studied drugs. The developed methods have been successfully used for determination of ATR and EZ in their combined dosage form and statistical comparison of the developed methods with the reported spectrophotometric one using F and Student's t-tests showed no significant difference regarding both accuracy and precision. PMID:29403754

Two spectrophotometric methods for simultaneous determination of some antihyperlipidemic drugs.

PubMed

Abdelwahab, Nada S; El-Zeiny, Badr A; Tohamy, Salwa I

2012-08-01

Two simple, accurate, precise and economic spectrophotometric methods have been developed for simultaneous determination of Atorvastatin calcium (ATR) and Ezetimibe (EZ) in their bulk powder and pharmaceutical dosage form. Method (I) is based on dual wavelength analysis while method (II) is the mean centering of ratio spectra spectrophotometric (MCR) method. In method (I), two wavelengths were selected for each drug in such a way that the difference in absorbance was zero for the second drug. At wavelengths 226.6 and 244 nm EZ had equal absorbance values; therefore, these two wavelengths have been used to determine ATR; on a similar basis 228.6 and 262.8 nm were selected to determine EZ in their binary mixtures. In method II, the absorption spectra of both ATR and EZ with different concentrations were recorded over the range 200-350, divided by the spectrum of suitable divisor of both ATR and EZ and then the obtained ratio spectra were mean centered. The concentrations of active components were then determined from the calibration graphs obtained by measuring the amplitudes at 215-260 nm (peak to peak) for both ATR and EZ. Accuracy and precision of the developed methods have been tested; in addition recovery studies have been carried out in order to confirm their accuracy. On the other hand, selectivities of the methods were tested by application for determination of different synthetic mixtures containing different ratios of the studied drugs. The developed methods have been successfully used for determination of ATR and EZ in their combined dosage form and statistical comparison of the developed methods with the reported spectrophotometric one using F and Student's t -tests showed no significant difference regarding both accuracy and precision.

Rapid spectrophotometric method for determining surface free energy of microalgal cells.

PubMed

Zhang, Xinru; Jiang, Zeyi; Li, Mengyin; Zhang, Xinxin; Wang, Ge; Chou, Aihui; Chen, Liang; Yan, Hai; Zuo, Yi Y

2014-09-02

Microalgae are one of the most promising renewable energy sources with environmental sustainability. The surface free energy of microalgal cells determines their biofouling and bioflocculation behavior and hence plays an important role in microalgae cultivation and harvesting. To date, the surface energetic properties of microalgal cells are still rarely studied. We developed a novel spectrophotometric method for directly determining the surface free energy of microalgal cells. The principles of this method are based on analyzing colloidal stability of microalgae suspensions. We have shown that this method can effectively differentiate the surface free energy of four microalgal strains, i.e., marine Chlorella sp., marine Nannochloris oculata, freshwater autotrophic Chlorella sp., and freshwater heterotrophic Chlorella sp. With advantages of high-throughput and simplicity, this new spectrophotometric method has the potential to evolve into a standard method for measuring the surface free energy of cells and abiotic particles.

A spectrophotometric method for detecting substellar companions to late-type M stars

NASA Astrophysics Data System (ADS)

Oetiker, Brian Glen

The most common stars in the Galaxy are the main-sequence M stars, yet current techniques are not optimized for detecting companions around the lowest mass stars; those with spectral designations ranging from M6 to M10. Described in this study is a search for companions around such stars using two methods: a unique implementation of the transit method, and a newly designed differential spectrophotometric method. The TEP project focusses on the detection of transits of terrestrial sized and larger companions in the eclipsing binary system CM Draconis. The newly designed spectrophotometric technique combines the strengths of the spectroscopic and photometric methods, while minimizing their inherent weaknesses. This unique method relies on the placement of three narrow band optical filters on and around the Titanium Oxide (TiO) bandhead near 8420 Å, a feature commonly seen in the atmospheres of late M stars. One filter is placed on the slope of the bandhead feature, while the remaining two are located on the adjacent continuum portions of the star's spectrum. The companion-induced motion of the star results in a doppler shifting of the bandhead feature, which in turn causes a change in flux passing through the filter located on the slope of the TiO bandhead. The spectrophotometric method is optimized for detecting compact systems containing brown dwarfs and giant planets. Because of its low dispersion-high photon efficiency design, this method is well suited for surveying large numbers of faint M stars. A small scale survey has been implemented, producing a candidate brown dwarf class companion of the star WX UMa. Applying the spectrophotometric method to a larger scale survey for brown dwarf and giant planet companions, coupled with a photometric transit study addresses two key astronomical issues. By detecting or placing limits on compact late type M star systems, a discrimination among competing theories of planetary formation may be gained. Furthermore, searching

Spectrophotometric and spectrofluorimetric methods for analysis of tramadol, acebutolol and dothiepin in pharmaceutical preparations

NASA Astrophysics Data System (ADS)

Abdellatef, Hisham E.; El-Henawee, Magda M.; El-Sayed, Heba M.; Ayad, Magda M.

2006-12-01

Sensitive spectrophotometric and spectrofluorimetric methods are described for the determination of tramadol, acebutolol and dothiepin (dosulepin) hydrochlorides. The two methods are based on the condensation of the cited drugs with the mixed anhydrides of malonic and acetic acids at 60 °C for 25-40 min. The coloured condensation products are suitable for the spectrophotometric and spectrofluorimetric determination at 329-333 and 431-434 nm (excitation at 389 nm), respectively. For the spectrophotometric method, Beer's law was obeyed from 0.5 to 2.5 μg ml -1 for tramadol, dothiepin and 5-25 μg ml -1 for acebutolol. Using the spectrofluorimetric method linearity ranged from 0.25 to 1.25 μg ml -1 for tramadol, dothiepin and 1-5 μg ml -1 for acebutolol. Mean percentage recoveries for the spectrophotometric method were 99.68 ± 1.00, 99.95 ± 1.11 and 99.72 ± 1.01 for tramadol, acebutolol and dothiepin, respectively and for the spectrofluorimetric method, recoveries were 99.5 ± 0.844, 100.32 ± 0.969 and 99.82 ± 1.15 for the three drugs, respectively. The optimum experimental parameters for the reaction has been studied. The validity of the described procedures was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed methods were successfully applied for the determination of the selected drugs in their pharmaceutical preparations with good recoveries. The procedures were accurate, simple and suitable for quality control application.

Validated spectrophotometric methods for determination of some oral hypoglycemic drugs.

PubMed

Farouk, M; Abdel-Satar, O; Abdel-Aziz, O; Shaaban, M

2011-02-01

Four accurate, precise, rapid, reproducible, and simple spectrophotometric methods were validated for determination of repaglinide (RPG), pioglitazone hydrochloride (PGL) and rosiglitazone maleate (RGL). The first two methods were based on the formation of a charge-transfer purple-colored complex of chloranilic acid with RPG and RGL with a molar absorptivity 1.23 × 10³ and 8.67 × 10² l•mol^-1•cm^-1 and a Sandell's sensitivity of 0.367 and 0.412 μg•cm^-2, respectively, and an ion-pair yellow-colored complex of bromophenol blue with RPG, PGL and RGL with molar absorptivity 8.86 × 10³, 6.95 × 10³, and 7.06 × 10³ l•mol^-1•cm^-1, respectively, and a Sandell's sensitivity of 0.051 μg•cm^-2 for all ion-pair complexes. The influence of different parameters on color formation was studied to determine optimum conditions for the visible spectrophotometric methods. The other spectrophotometric methods were adopted for demtermination of the studied drugs in the presence of their acid-, alkaline- and oxidative-degradates by computing derivative and pH-induced difference spectrophotometry, as stability-indicating techniques. All the proposed methods were validated according to the International Conference on Harmonization guidelines and successfully applied for determination of the studied drugs in pure form and in pharmaceutical preparations with good extraction recovery ranges between 98.7-101.4%, 98.2-101.3%, and 99.9-101.4% for RPG, PGL, and RGL, respectively. Results of relative standard deviations did not exceed 1.6%, indicating that the proposed methods having good repeatability and reproducibility. All the obtained results were statistically compared to the official method used for RPG analysis and the manufacturers methods used for PGL and RGL analysis, respectively, where no significant differences were found.

Spectrophotometric methods for the determination of urea in real samples using silver nanoparticles by standard addition and 2nd order derivative methods

NASA Astrophysics Data System (ADS)

Ali, Nauman; Ismail, Muhammad; Khan, Adnan; Khan, Hamayun; Haider, Sajjad; Kamal, Tahseen

2018-01-01

In this work, we have developed simple, sensitive and inexpensive methods for the spectrophotometric determination of urea in urine samples using silver nanoparticles (AgNPs). The standard addition and 2nd order derivative methods were adopted for this purpose. AgNPs were prepared by chemical reduction of AgNO3 with hydrazine using 1,3-di-(1H-imidazol-1-yl)-2-propanol (DIPO) as a stabilizing agent in aqueous medium. The proposed methods were based on the complexation of AgNPs with urea. Using this concept, urea in the urine samples was successfully determined spectrophotometric methods. The results showed high percent recovery with ± RSD. The recoveries of urea in the three urine samples by spectrophotometric standard addition were 99.2% ± 5.37, 96.3% ± 4.49, 104.88% ± 4.99 and that of spectrophotometric 2nd order derivative method were 115.3% ± 5.2, 103.4% ± 2.6, 105.93% ± 0.76. The results show that these methods can open doors for a potential role of AgNPs in the clinical determination of urea in urine, blood, biological, non-biological fluids.

Evaluation of ultraviolet spectrophotometry for simultaneous analysis of alkylbenzenes, alkylnaphthalenes, alkylanthracenes/phenanthrenes and total aromatics in mid-distillate fuels

NASA Technical Reports Server (NTRS)

Kim, W. S.; Seng, G. T.

1982-01-01

A rapid ultraviolet spectrophotometric method for the simultaneous determination of aromatics in middistillate fuels was developed and evaluated. In this method, alkylbenzenes, alkylnaphthalenes, alkylanthracenes/phenanthracenes and total aromatics were determined from ultraviolet spectra of the fuels. The accuracy and precision were determined using simulated standard fuels with known compositions. The total aromatics fraction accuracy was 5% for a Jet A type fuel and 0.6% for a broadened properties jet turbine type fuel. Precision, expressed as relative standard deviations, ranged from 2.9% for the alkylanthracenes/phenanthrenes to 15.3% for the alkylbenzenes. The accuracy, however, was less for actual fuel samples when compared to the results obtained by a mass spectrometric method. In addition, the ASTM D-1840 method for naphthalenes by ultraviolet spectroscopy was evaluated.

A continuous spectrophotometric assay method for peptidylarginine deiminase type 4 activity.

PubMed

Liao, Ya-Fan; Hsieh, Hui-Chieh; Liu, Guang-Yaw; Hung, Hui-Chih

2005-12-15

A simple, continuous spectrophotometric assay for peptidylarginine deiminase (PAD) is described. Deimination of peptidylarginine results in the formation of peptidylcitrulline and ammonia. The ammonia released during peptidylarginine hydrolysis is coupled to the glutamate-dehydrogenase-catalyzed reductive amination of alpha-ketoglutarate to glutamate and reduced nicotinamide adenine dinucleotide (NADH) oxidation. The disappearance of absorbance at 340nm due to NADH oxidation is continuously measured. The specific activity obtained by this new protocol for highly purified human PAD is comparable to that obtained by a commonly used colorimetric procedure, which measures the ureido group of peptidylcitrulline by coupling with diacetyl monoxime. The present continuous spectrophotometric method is highly sensitive and accurate and is thus suitable for enzyme kinetic analysis of PAD. The Ca(2+) concentration for half-maximal activity of PAD obtained by this method is comparable to that previously obtained by the colorimetric procedure.

Spectrophotometric observations of symbiotic stars and related objects

NASA Technical Reports Server (NTRS)

Blair, W. P.; Feibelman, W. A.; Michalitsianos, A. G.; Stencel, R. E.

1983-01-01

Calibrated optical spectrophotometric observations of 16 symbiotic and symbiotic-like objects are presented. The objects observed include Z And, T CrB, CH Cyg, CI Cyg, V1016 Cyg, V1329 Cyg, AG Dra, YY Her, RS Oph, XX Oph, AG Peg, AX Per, CL Sco, HM Sge, AS 289, and M1-2. Integrated emission-line intensities are tabulated for comparison with ultraviolet and infrared data, as well as with previous optical studies. The reddening to each of the objects is derived by assuming that Balmer lines are emitted in their case B recombination ratios. However, the values so derived are often systematically higher than reddening estimates from the ultraviolet 2200 A feature. Comparisons with the available data from other wavelength ranges are noted.

Spectrophotometric Analysis of Caffeine

PubMed Central

Ahmad Bhawani, Showkat; Fong, Sim Siong; Mohamad Ibrahim, Mohamad Nasir

2015-01-01

The nature of caffeine reveals that it is a bitter white crystalline alkaloid. It is a common ingredient in a variety of drinks (soft and energy drinks) and is also used in combination with various medicines. In order to maintain the optimum level of caffeine, various spectrophotometric methods have been developed. The monitoring of caffeine is very important aspect because of its consumption in higher doses that can lead to various physiological disorders. This paper incorporates various spectrophotometric methods used in the analysis of caffeine in various environmental samples such as pharmaceuticals, soft and energy drinks, tea, and coffee. A range of spectrophotometric methodologies including chemometric techniques and derivatization of spectra have been used to analyse the caffeine. PMID:26604926

AN ULTRAVIOLET-VISIBLE SPECTROPHOTOMETER AUTOMATION SYSTEM. PART III: PROGRAM DOCUMENTATION

EPA Science Inventory

The Ultraviolet-Visible Spectrophotometer (UVVIS) automation system accomplishes 'on-line' spectrophotometric quality assurance determinations, report generations, plot generations and data reduction for chlorophyll or color analysis. This system also has the capability to proces...

Different Spectrophotometric and Chromatographic Methods for Determination of Mepivacaine and Its Toxic Impurity.

PubMed

Abdelwahab, Nada S; Fared, Nehal F; Elagawany, Mohamed; Abdelmomen, Esraa H

2017-09-01

Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.

Spectrophotometric and Reversed-Phase High-Performance Liquid Chromatographic Method for the Determination of Doxophylline in Pharmaceutical Formulations

PubMed Central

Joshi, HR; Patel, AH; Captain, AD

2010-01-01

Two methods are described for determination of Doxophylline in a solid dosage form. The first method was based on ultraviolet (UV)-spectrophotometric determination of the drug. It involves absorbance measurement at 274 nm (λmax of Doxophylline) in 0.1 N hydrochloric acid. The calibration curve was linear, with the correlation coefficient between 0.99 and 1.0 over a concentration range of 0.20–30 mg/ml for the drug. The second method was based on high-performance liquid chromatography (HPLC) separation of the drug in reverse-phase mode using the Hypersil ODS C18 column (250 × 4.6 mm, 5 mm). The mobile phase constituted of buffer acetonitrile (80:20) and pH adjusted to 3.0, with dilute orthophosphoric acid delivered at a flow rate 1.0 ml/min. Detection was performed at 210 nm. Separation was completed within 7 min. The calibration curve was linear, with the correlation coefficient between 0.99 and 1.0 over a concentration range of 0.165–30 mg/ml for the drug. The relative standard deviation was found to be <2.0% for the UV-spectrophotometry and HPLC methods. Both these methods have been successively applied to the solid dosage pharmaceutical formulation, and were fully validated according to ICH guidelines. PMID:21042488

REVIEW ARTICLE: Spectrophotometric applications of digital signal processing

NASA Astrophysics Data System (ADS)

Morawski, Roman Z.

2006-09-01

Spectrophotometry is more and more often the method of choice not only in analysis of (bio)chemical substances, but also in the identification of physical properties of various objects and their classification. The applications of spectrophotometry include such diversified tasks as monitoring of optical telecommunications links, assessment of eating quality of food, forensic classification of papers, biometric identification of individuals, detection of insect infestation of seeds and classification of textiles. In all those applications, large numbers of data, generated by spectrophotometers, are processed by various digital means in order to extract measurement information. The main objective of this paper is to review the state-of-the-art methodology for digital signal processing (DSP) when applied to data provided by spectrophotometric transducers and spectrophotometers. First, a general methodology of DSP applications in spectrophotometry, based on DSP-oriented models of spectrophotometric data, is outlined. Then, the most important classes of DSP methods for processing spectrophotometric data—the methods for DSP-aided calibration of spectrophotometric instrumentation, the methods for the estimation of spectra on the basis of spectrophotometric data, the methods for the estimation of spectrum-related measurands on the basis of spectrophotometric data—are presented. Finally, the methods for preprocessing and postprocessing of spectrophotometric data are overviewed. Throughout the review, the applications of DSP are illustrated with numerous examples related to broadly understood spectrophotometry.

Compatible validated spectrofluorimetric and spectrophotometric methods for determination of vildagliptin and saxagliptin by factorial design experiments.

PubMed

Abdel-Aziz, Omar; Ayad, Miriam F; Tadros, Mariam M

2015-04-05

Simple, selective and reproducible spectrofluorimetric and spectrophotometric methods have been developed for the determination of vildagliptin and saxagliptin in bulk and their pharmaceutical dosage forms. The first proposed spectrofluorimetric method is based on the dansylation reaction of the amino group of vildagliptin with dansyl chloride to form a highly fluorescent product. The formed product was measured spectrofluorimetrically at 455 nm after excitation at 345 nm. Beer's law was obeyed in a concentration range of 100-600 μg ml(-1). The second proposed spectrophotometric method is based on the charge transfer complex of saxagliptin with tetrachloro-1,4-benzoquinone (p-chloranil). The formed charge transfer complex was measured spectrophotometrically at 530 nm. Beer's law was obeyed in a concentration range of 100-850 μg ml(-1). The third proposed spectrophotometric method is based on the condensation reaction of the primary amino group of saxagliptin with formaldehyde and acetyl acetone to form a yellow colored product known as Hantzsch reaction, measured at 342.5 nm. Beer's law was obeyed in a concentration range of 50-300 μg ml(-1). All the variables were studied to optimize the reactions' conditions using factorial design. The developed methods were validated and proved to be specific and accurate for quality control of vildagliptin and saxagliptin in their pharmaceutical dosage forms. Copyright © 2015. Published by Elsevier B.V.

Compatible validated spectrofluorimetric and spectrophotometric methods for determination of vildagliptin and saxagliptin by factorial design experiments

NASA Astrophysics Data System (ADS)

Abdel-Aziz, Omar; Ayad, Miriam F.; Tadros, Mariam M.

2015-04-01

Simple, selective and reproducible spectrofluorimetric and spectrophotometric methods have been developed for the determination of vildagliptin and saxagliptin in bulk and their pharmaceutical dosage forms. The first proposed spectrofluorimetric method is based on the dansylation reaction of the amino group of vildagliptin with dansyl chloride to form a highly fluorescent product. The formed product was measured spectrofluorimetrically at 455 nm after excitation at 345 nm. Beer's law was obeyed in a concentration range of 100-600 μg ml-1. The second proposed spectrophotometric method is based on the charge transfer complex of saxagliptin with tetrachloro-1,4-benzoquinone (p-chloranil). The formed charge transfer complex was measured spectrophotometrically at 530 nm. Beer's law was obeyed in a concentration range of 100-850 μg ml-1. The third proposed spectrophotometric method is based on the condensation reaction of the primary amino group of saxagliptin with formaldehyde and acetyl acetone to form a yellow colored product known as Hantzsch reaction, measured at 342.5 nm. Beer's law was obeyed in a concentration range of 50-300 μg ml-1. All the variables were studied to optimize the reactions' conditions using factorial design. The developed methods were validated and proved to be specific and accurate for quality control of vildagliptin and saxagliptin in their pharmaceutical dosage forms.

Simultaneous determination of some cholesterol-lowering drugs in their binary mixture by novel spectrophotometric methods

NASA Astrophysics Data System (ADS)

Lotfy, Hayam Mahmoud; Hegazy, Maha Abdel Monem

2013-09-01

Four simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of simvastatin (SM) and ezetimibe (EZ) namely; extended ratio subtraction (EXRSM), simultaneous ratio subtraction (SRSM), ratio difference (RDSM) and absorption factor (AFM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated and the specificity was assessed by analyzing synthetic mixtures containing the cited drugs. The four methods were applied for the determination of the cited drugs in tablets and the obtained results were statistically compared with each other and with those of a reported HPLC method. The comparison showed that there is no significant difference between the proposed methods and the reported method regarding both accuracy and precision.

Automated spectrophotometric bicarbonate analysis in duodenal juice compared to the back titration method.

PubMed

Erchinger, Friedemann; Engjom, Trond; Gudbrandsen, Oddrun Anita; Tjora, Erling; Gilja, Odd H; Dimcevski, Georg

2016-01-01

We have recently evaluated a short endoscopic secretin test for exocrine pancreatic function. Bicarbonate concentration in duodenal juice is an important parameter in this test. Measurement of bicarbonate by back titration as the gold standard method is time consuming, expensive and technically difficult, thus a simplified method is warranted. We aimed to evaluate an automated spectrophotometric method in samples spanning the effective range of bicarbonate concentrations in duodenal juice. We also evaluated if freezing of samples before analyses would affect its results. Patients routinely examined with short endoscopic secretin test suspected to have decreased pancreatic function of various reasons were included. Bicarbonate in duodenal juice was quantified by back titration and automatic spectrophotometry. Both fresh and thawed samples were analysed spectrophotometrically. 177 samples from 71 patients were analysed. Correlation coefficient of all measurements was r = 0.98 (p < 0.001). Correlation coefficient of fresh versus frozen samples conducted with automatic spectrophotometry (n = 25): r = 0.96 (p < 0.001) CONCLUSIONS: The measurement of bicarbonate in fresh and thawed samples by automatic spectrophotometrical analysis correlates excellent with the back titration gold standard. This is a major simplification of direct pancreas function testing, and allows a wider distribution of bicarbonate testing in duodenal juice. Extreme values for Bicarbonate concentration achieved by the autoanalyser method have to be interpreted with caution. Copyright © 2016 IAP and EPC. Published by Elsevier India Pvt Ltd. All rights reserved.

Quantitative determination of zopiclone and its impurity by four different spectrophotometric methods.

PubMed

Abdelrahman, Maha M; Naguib, Ibrahim A; El Ghobashy, Mohamed R; Ali, Nesma A

2015-02-25

Four simple, sensitive and selective spectrophotometric methods are presented for determination of Zopiclone (ZPC) and its impurity, one of its degradation products, namely; 2-amino-5-chloropyridine (ACP). Method A is a dual wavelength spectrophotometry; where two wavelengths (252 and 301 nm for ZPC, and 238 and 261 nm for ACP) were selected for each component in such a way that difference in absorbance is zero for the second one. Method B is isoabsorptive ratio method by combining the isoabsorptive point (259.8 nm) in the ratio spectrum using ACP as a divisor and the ratio difference for a single step determination of both components. Method C is third derivative (D(3)) spectrophotometric method which allows determination of both ZPC at 283.6 nm and ACP at 251.6 nm without interference of each other. Method D is based on measuring the peak amplitude of the first derivative of the ratio spectra (DD(1)) at 263.2 nm for ZPC and 252 nm for ACP. The suggested methods were validated according to ICH guidelines and can be applied for routine analysis in quality control laboratories. Statistical analysis of the results obtained from the proposed methods and those obtained from the reported method has been carried out revealing high accuracy and good precision. Copyright © 2014 Elsevier B.V. All rights reserved.

Spectrophotometric Investigations of Macrolide Antibiotics: A Brief Review

PubMed Central

Keskar, Mrudul R; Jugade, Ravin M

2015-01-01

Macrolides, one of the most commonly used class of antibiotics, are a group of drugs produced by Streptomyces species. They belong to the polyketide class of natural products. Their activity is due to the presence of a large macrolide lactone ring with deoxy sugar moieties. They are protein synthesis inhibitors and broad-spectrum antibiotics, active against both gram-positive and gram-negative bacteria. Different analytical techniques have been reported for the determination of macrolides such as chromatographic methods, flow injection methods, spectrofluorometric methods, spectrophotometric methods, and capillary electrophoresis methods. Among these methods, spectrophotometric methods are sensitive and cost effective for the analysis of various antibiotics in pharmaceutical formulations as well as biological samples. This article reviews different spectrophotometric methods for the determination of macrolide antibiotics. PMID:26609215

Validated chromatographic and spectrophotometric methods for analysis of some amoebicide drugs in their combined pharmaceutical preparation.

PubMed

Abdelaleem, Eglal Adelhamid; Abdelwahab, Nada Sayed

2013-01-01

This work is concerned with development and validation of chromatographic and spectrophotometric methods for analysis of mebeverine HCl (MEH), diloxanide furoate (DF) and metronidazole (MET) in Dimetrol® tablets - spectrophotometric and RP-HPLC methods using UV detection. The developed spectrophotometric methods depend on determination of MEH and DF in the combined dosage form using the successive derivative ratio spectra method which depends on derivatization of the obtained ratio spectra in two steps using methanol as a solvent and measuring MEH at 226.4-232.2 nm (peak to peak) and DF at 260.6-264.8 nm (peak to peak). While MET concentrations were determined using first derivative (1D) at λ = 327 nm using the same solvent. The chromatographic method depends on HPLC separation on ODS column and elution with a mobile phase consisting water: methanol: triethylamine (25: 75: 0.5, by volume, orthophosphoric acid to pH =4). Pumping the mobile phase at 0.7 ml min-1 with UV at 230 nm. Factors affecting the developed methods were studied and optimized, moreover, they have been validated as per ICH guideline and the results demonstrated that the suggested methods are reproducible, reliable and can be applied for routine use with short time of analysis. Statistical analysis of the two developed methods with each other using F and student's-t tests showed no significant difference.

Method for extreme ultraviolet lithography

DOEpatents

Felter, T. E.; Kubiak, Glenn D.

1999-01-01

A method of producing a patterned array of features, in particular, gate apertures, in the size range 0.4-0.05 .mu.m using projection lithography and extreme ultraviolet (EUV) radiation. A high energy laser beam is used to vaporize a target material in order to produce a plasma which in turn, produces extreme ultraviolet radiation of a characteristic wavelength of about 13 nm for lithographic applications. The radiation is transmitted by a series of reflective mirrors to a mask which bears the pattern to be printed. The demagnified focused mask pattern is, in turn, transmitted by means of appropriate optics and in a single exposure, to a substrate coated with photoresists designed to be transparent to EUV radiation and also satisfy conventional processing methods.

Method for extreme ultraviolet lithography

DOEpatents

Felter, T. E.; Kubiak, G. D.

2000-01-01

A method of producing a patterned array of features, in particular, gate apertures, in the size range 0.4-0.05 .mu.m using projection lithography and extreme ultraviolet (EUV) radiation. A high energy laser beam is used to vaporize a target material in order to produce a plasma which in turn, produces extreme ultraviolet radiation of a characteristic wavelength of about 13 nm for lithographic applications. The radiation is transmitted by a series of reflective mirrors to a mask which bears the pattern to be printed. The demagnified focused mask pattern is, in turn, transmitted by means of appropriate optics and in a single exposure, to a substrate coated with photoresists designed to be transparent to EUV radiation and also satisfy conventional processing methods.

Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation.

PubMed

Merey, Hanan A; Abd-Elmonem, Mahmmoud S; Nazlawy, Hagar N; Zaazaa, Hala E

2017-01-01

Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY) and Flunixin Meglumine (FLU). The first method, dual wavelength (DW), depends on measuring the difference in absorbance (ΔA 273.4-327 nm) for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7-275.7 nm. The second method, first-derivative spectrophotometric method (1D), depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5-324.8 nm and ΔP 249.6-286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD), depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones.

Spectrophotometric and HPLC Methods for Simultaneous Estimation of Amlodipine Besilate, Losartan Potassium and Hydrochlorothiazide in Tablets

PubMed Central

Wankhede, S. B.; Raka, K. C.; Wadkar, S. B.; Chitlange, S. S.

2010-01-01

Two UV-spectrophotometric and one reverse phase high performance liquid chromatography methods have been developed for the simultaneous estimation of amlodipine besilate, losartan potassium and hydrochlorothiazide in tablet dosage form. The first UV spectrophotometric method was a determination using the simultaneous equation method at 236.5, 254 and 271 nm over the concentration range 5-25, 10-50 and 5-25 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. The second UV method was a determination using the area under curve method at 231.5-241.5, 249-259 and 266-276 nm over the concentration range of 5-25, 5-25 and 10-50 μg/ml for amlodipine besilate, hydrochlorothiazide and losartan potassium, respectively. In reverse phase high performance liquid chromatography analysis is carried out using 0.025 M phosphate buffer (pH 3.7):acetonitrile (57:43 v/v) as the mobile phase and Kromasil C18 (4.6 mm i.d×250 mm) column as stationery phase with detection wavelength of 232 nm linearity was obtained in the concentration range of 2-14, 20-140 and 5-40 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. Both UV-spectrophotometric and reverse phase high performance liquid chromatography methods were statistically validated and can be used for analysis of combined dose tablet formulation containing amlodipine besilate, losartan potassium and hydrochlorothiazide. PMID:20582208

Flow injection spectrophotometric method for chloride determination in natural waters using Hg(SCN)(2) immobilized in epoxy resin.

PubMed

Silva, Claudineia R; Vieira, Heberth J; Canaes, Larissa S; Nóbrega, Joaquim A; Fatibello-Filho, Orlando

2005-02-28

A flow injection (FI) spectrophotometric method was proposed for the determination of chloride ion in natural waters. The determination of chloride was carried out by reaction with Hg(SCN)(2) immobilized in an epoxy resin bead in a solid-phase reactor (SPR) and the thiocyanate ions released were determined spectrophotometrically at 480nm after complexing reaction with Fe(III). The analytical curve for chloride was linear in the concentration range from 5.6 x 10(-5) to 2.2 x 10(-4)moll(-1) with a detection limit of 1.4 x 10(-5)moll(-1). The relative standard deviation (R.S.D.) was 2.2% for a solution containing 2.2 x 10(-4)moll(-1) (n = 10). The simple manifold allows a routine analytical frequency of 100 determinations per hour. The main advantage of the developed method is the 400% reduction of the Hg waste solution generated when compared to conventional methods for chloride determination based on the same spectrophotometric reaction.

Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

NASA Astrophysics Data System (ADS)

Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

2017-02-01

A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

Determination of lead and cadmium in soils, sludges, and fertilizers by an ion-exchange/spectrophotometric method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heinzig, M.; DeYong, G.D.; Anglin, R.J.

1993-12-01

The MetalTrace method, which consists of an anion-exchange separation coupled with a spectrophotometric quantification, was used to determine lead and cadmium in sulfuric acid-hydrogen peroxide digests of soils and sludges and hydrobromic acid extracts of soils. Cadmium only was determined in sulfuric acid-hydrogen peroxide digests of fertilizers because no standards were available with certified lead contents. The selectivity provided by the anion-exchange separation allowed the use of a spectrophotometric indicator with an extremely high extinction coefficient so that detection limits in the low parts per million range could be attained. The results obtained using this method compared favorably with thosemore » obtained using much more expensive methods requiring more specialized training and equipment.« less

Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation

PubMed Central

Abd-Elmonem, Mahmmoud S.; Nazlawy, Hagar N.; Zaazaa, Hala E.

2017-01-01

Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY) and Flunixin Meglumine (FLU). The first method, dual wavelength (DW), depends on measuring the difference in absorbance (ΔA 273.4–327 nm) for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7–275.7 nm. The second method, first-derivative spectrophotometric method (1D), depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5–324.8 nm and ΔP 249.6–286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD), depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones. PMID:28811956

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

PubMed

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Computation of geometric representation of novel spectrophotometric methods used for the analysis of minor components in pharmaceutical preparations.

PubMed

Lotfy, Hayam M; Saleh, Sarah S; Hassan, Nagiba Y; Salem, Hesham

2015-01-01

Novel spectrophotometric methods were applied for the determination of the minor component tetryzoline HCl (TZH) in its ternary mixture with ofloxacin (OFX) and prednisolone acetate (PA) in the ratio of (1:5:7.5), and in its binary mixture with sodium cromoglicate (SCG) in the ratio of (1:80). The novel spectrophotometric methods determined the minor component (TZH) successfully in the two selected mixtures by computing the geometrical relationship of either standard addition or subtraction. The novel spectrophotometric methods are: geometrical amplitude modulation (GAM), geometrical induced amplitude modulation (GIAM), ratio H-point standard addition method (RHPSAM) and compensated area under the curve (CAUC). The proposed methods were successfully applied for the determination of the minor component TZH below its concentration range. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed. No difference was observed between the obtained results when compared to the reported HPLC method, which proved that the developed methods could be alternative to HPLC techniques in quality control laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Spectrophotometric methods for simultaneous determination of betamethasone valerate and fusidic acid in their binary mixture.

PubMed

Lotfy, Hayam Mahmoud; Salem, Hesham; Abdelkawy, Mohammad; Samir, Ahmed

2015-04-05

Five spectrophotometric methods were successfully developed and validated for the determination of betamethasone valerate and fusidic acid in their binary mixture. Those methods are isoabsorptive point method combined with the first derivative (ISO Point--D1) and the recently developed and well established methods namely ratio difference (RD) and constant center coupled with spectrum subtraction (CC) methods, in addition to derivative ratio (1DD) and mean centering of ratio spectra (MCR). New enrichment technique called spectrum addition technique was used instead of traditional spiking technique. The proposed spectrophotometric procedures do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analyzing synthetic mixtures of both drugs. They were applied to their pharmaceutical formulation and the results obtained were statistically compared to that of official methods. The statistical comparison showed that there is no significant difference between the proposed methods and the official ones regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Validated spectrophotometric methods for determination of Alendronate sodium in tablets through nucleophilic aromatic substitution reactions

PubMed Central

2012-01-01

Background Alendronate (ALD) is a member of the bisphosphonate family which is used for the treatment of osteoporosis, bone metastasis, Paget's disease, hypocalcaemia associated with malignancy and other conditions that feature bone fragility. ALD is a non-chromophoric compound so its determination by conventional spectrophotometric methods is not possible. So two derivatization reactions were proposed for determination of ALD through the reaction with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) and 2,4-dinitrofluorobenzene (DNFB) as chromogenic derivatizing reagents. Results Three simple and sensitive spectrophotometric methods are described for the determination of ALD. Method I is based on the reaction of ALD with NBD-Cl. Method II involved heat-catalyzed derivatization of ALD with DNFB, while, Method III is based on micellar-catalyzed reaction of the studied drug with DNFB at room temperature. The reactions products were measured at 472, 378 and 374 nm, for methods I, II and III, respectively. Beer's law was obeyed over the concentration ranges of 1.0-20.0, 4.0-40.0 and 1.5-30.0 μg/mL with lower limits of detection of 0.09, 1.06 and 0.06 μg/mL for Methods I, II and III, respectively. The proposed methods were applied for quantitation of the studied drug in its pure form with mean percentage recoveries of 100.47 ± 1.12, 100.17 ± 1.21 and 99.23 ± 1.26 for Methods I, II and III, respectively. Moreover the proposed methods were successfully applied for determination of ALD in different tablets. Proposals of the reactions pathways have been postulated. Conclusion The proposed spectrophotometric methods provided sensitive, specific and inexpensive analytical procedures for determination of the non-chromophoric drug alendronate either per se or in its tablet dosage forms without interference from common excipients. Graphical abstract PMID:22472190

Validated spectrophotometric methods for determination of Alendronate sodium in tablets through nucleophilic aromatic substitution reactions.

PubMed

Walash, Mohamed I; Metwally, Mohamed E-S; Eid, Manal; El-Shaheny, Rania N

2012-04-02

Alendronate (ALD) is a member of the bisphosphonate family which is used for the treatment of osteoporosis, bone metastasis, Paget's disease, hypocalcaemia associated with malignancy and other conditions that feature bone fragility. ALD is a non-chromophoric compound so its determination by conventional spectrophotometric methods is not possible. So two derivatization reactions were proposed for determination of ALD through the reaction with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) and 2,4-dinitrofluorobenzene (DNFB) as chromogenic derivatizing reagents. Three simple and sensitive spectrophotometric methods are described for the determination of ALD. Method I is based on the reaction of ALD with NBD-Cl. Method II involved heat-catalyzed derivatization of ALD with DNFB, while, Method III is based on micellar-catalyzed reaction of the studied drug with DNFB at room temperature. The reactions products were measured at 472, 378 and 374 nm, for methods I, II and III, respectively. Beer's law was obeyed over the concentration ranges of 1.0-20.0, 4.0-40.0 and 1.5-30.0 μg/mL with lower limits of detection of 0.09, 1.06 and 0.06 μg/mL for Methods I, II and III, respectively. The proposed methods were applied for quantitation of the studied drug in its pure form with mean percentage recoveries of 100.47 ± 1.12, 100.17 ± 1.21 and 99.23 ± 1.26 for Methods I, II and III, respectively. Moreover the proposed methods were successfully applied for determination of ALD in different tablets. Proposals of the reactions pathways have been postulated. The proposed spectrophotometric methods provided sensitive, specific and inexpensive analytical procedures for determination of the non-chromophoric drug alendronate either per se or in its tablet dosage forms without interference from common excipients. GRAPHICAL

Reduction of ultraviolet transmission through cotton T-shirt fabrics with low ultraviolet protection by various laundering methods and dyeing: clinical implications.

PubMed

Wang, S Q; Kopf, A W; Marx, J; Bogdan, A; Polsky, D; Bart, R S

2001-05-01

The public has long been instructed to wear protective clothing against ultraviolet (UV) damage. Our purpose was to determine the UV protection factor (UPF) of two cotton fabrics used in the manufacture of summer T-shirts and to explore methods that could improve the UPF of these fabrics. Each of the two types of white cotton fabrics (cotton T-shirt and mercerized cotton print cloth) used in this study was divided into 4 treatment groups: (1) water-only (machine washed with water), (2) detergent-only (washed with detergent), (3) detergent-UV absorber (washed with detergent and a UV absorber), and (4) dyes (dyed fabrics). Ultraviolet transmission through the fabrics was measured with a spectrophotometer before and after laundry and dyeing treatments. Based on UV transmission through these fabrics, the UPF values were calculated. Before any treatments, the mean UPFs were 4.94 for the T-shirt fabric and 3.13 for the print cloth. There was greater UVA (320-400 nm) than UVB (280-320 nm) transmission through these fabrics. After 5 washings with water alone and with detergent alone, UPF increased by 51% and 17%, respectively, for the cotton T-shirt fabric. Washing the T-shirt fabrics with detergent plus the UV-absorbing agent increased the UPF by 407% after 5 treatments. Dyeing the fabric blue or yellow increased the UPF by 544% and 212%, respectively. Similar changes in UPFs were observed for the print cloth fabric. The two cotton fabrics used in this study offered limited protection against UV radiation as determined by spectrophotometric analysis. Laundering with detergent and water improves UPF slightly by causing fabric shrinkage. Dyeing fabrics or adding a UV-absorbing agent during laundering substantially reduces UV transmission and increases UPF. More UVA is transmitted through the fabrics than UVB.

Validated univariate and multivariate spectrophotometric methods for the determination of pharmaceuticals mixture in complex wastewater

NASA Astrophysics Data System (ADS)

Riad, Safaa M.; Salem, Hesham; Elbalkiny, Heba T.; Khattab, Fatma I.

2015-04-01

Five, accurate, precise, and sensitive univariate and multivariate spectrophotometric methods were developed for the simultaneous determination of a ternary mixture containing Trimethoprim (TMP), Sulphamethoxazole (SMZ) and Oxytetracycline (OTC) in waste water samples collected from different cites either production wastewater or livestock wastewater after their solid phase extraction using OASIS HLB cartridges. In univariate methods OTC was determined at its λmax 355.7 nm (0D), while (TMP) and (SMZ) were determined by three different univariate methods. Method (A) is based on successive spectrophotometric resolution technique (SSRT). The technique starts with the ratio subtraction method followed by ratio difference method for determination of TMP and SMZ. Method (B) is successive derivative ratio technique (SDR). Method (C) is mean centering of the ratio spectra (MCR). The developed multivariate methods are principle component regression (PCR) and partial least squares (PLS). The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures containing different ratios of the three drugs. The obtained results are statistically compared with those obtained by the official methods, showing no significant difference with respect to accuracy and precision at p = 0.05.

Validated univariate and multivariate spectrophotometric methods for the determination of pharmaceuticals mixture in complex wastewater.

PubMed

Riad, Safaa M; Salem, Hesham; Elbalkiny, Heba T; Khattab, Fatma I

2015-04-05

Five, accurate, precise, and sensitive univariate and multivariate spectrophotometric methods were developed for the simultaneous determination of a ternary mixture containing Trimethoprim (TMP), Sulphamethoxazole (SMZ) and Oxytetracycline (OTC) in waste water samples collected from different cites either production wastewater or livestock wastewater after their solid phase extraction using OASIS HLB cartridges. In univariate methods OTC was determined at its λmax 355.7 nm (0D), while (TMP) and (SMZ) were determined by three different univariate methods. Method (A) is based on successive spectrophotometric resolution technique (SSRT). The technique starts with the ratio subtraction method followed by ratio difference method for determination of TMP and SMZ. Method (B) is successive derivative ratio technique (SDR). Method (C) is mean centering of the ratio spectra (MCR). The developed multivariate methods are principle component regression (PCR) and partial least squares (PLS). The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures containing different ratios of the three drugs. The obtained results are statistically compared with those obtained by the official methods, showing no significant difference with respect to accuracy and precision at p=0.05. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of the brand new two-drug combination for the treatment of hepatitis C: Sofosbuvir/ledipasvir using smart spectrophotometric methods manipulating ratio spectra

NASA Astrophysics Data System (ADS)

Eissa, Maya S.

2017-08-01

In this work, various sensitive and selective spectrophotometric methods were first introduced for the simultaneous determination of sofosbuvir and ledipasvir in their binary mixture without preliminary separation. Ledipasvir was determined simply by zero-order spectrophotometric method at its λmax = 333.0 nm in a linear range of 2.5-30.0 μg/ml without any interference of sofosbuvir even in low or high concentrations and with mean percentage recovery of 100.05 ± 0.632. Sofosbuvir can be quantitatively estimated by one of the following smart spectrophotometric methods based on ratio spectra developed for the resolution of the overlapped spectra of their binary mixture; ratio difference spectrophotometric method (RD) by computing the difference between the amplitudes of sofosbuvir ratio spectra at 228 nm and 270 nm, first derivative (DD1) of ratio spectra by measuring the sum of amplitude of trough and peak at 265 nm and 277 nm, respectively, ratio subtraction (RS) spectrophotometric method in which sofosbuvir can be successfully determined at its λmax = 261.0 nm and mean centering (MC) of ratio spectra by measuring the mean centering values at 270 nm. All of the above mentioned spectrophotometric methods can estimate sofosbuvir in a linear range of 7.5-90.0 μg/ml with mean percentage recoveries of 100.57 ± 0.810, 99.92 ± 0.759, 99.51 ± 0.475 and 100.75 ± 0.672, respectively. These methods were successfully applied to the analysis of their combined dosage form and bulk powder. The adopted methods were also validated as per ICH guidelines and statistically compared to an in-house HPLC method.

Determination of niobium in rocks by an isotope dilution spectrophotometric method

USGS Publications Warehouse

Greenland, L.P.; Campbell, E.Y.

1970-01-01

Rocks and minerals are fused with sodium peroxide in the presence of carrierfree 95Nb. The fusion cake is leached with water and the precipitate dissolved in hydrofluoric-sulfuric acid mixture. Niobium is extracted into methyl isobutyl ketone and further purified by ion exchange. The amount of niobium is determined spectrophotometrically with 4-(2-pyridylazo)-resorcinol, and the chemical yield of the separations determined by counting 95Nb. This procedure is faster and less sensitive to interferences than previously proposed methods for determining niobium in rocks.The high purity of the separated niobium makes the method applicable to nearly all matrices. ?? 1970.

Development and validation of spectrophotometric, atomic absorption and kinetic methods for determination of moxifloxacin hydrochloride.

PubMed

Abdellaziz, Lobna M; Hosny, Mervat M

2011-01-01

Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe(3+) ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2' bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange-red ion-pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8-6, 0.8-4) for methods A and B, (16-96, 16-96 and 16-72) for procedures 1-3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical formulations

Development and Validation of Spectrophotometric, Atomic Absorption and Kinetic Methods for Determination of Moxifloxacin Hydrochloride

PubMed Central

Abdellaziz, Lobna M.; Hosny, Mervat M.

2011-01-01

Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe3+ ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2′ bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange—red ion-pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8–6, 0.8–4) for methods A and B, (16–96, 16–96 and 16–72) for procedures 1–3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical

Method for removal of phosgene from boron trichloride

DOEpatents

Freund, Samuel M.

1983-01-01

Selective ultraviolet photolysis using an unfiltered mercury arc lamp has been used to substantially reduce the phosgene impurity in a mixture of boron trichloride and phosgene. Infrared spectrophotometric analysis of the sample before and after irradiation shows that is is possible to highly purify commercially available boron trichloride with this method.

Novel two wavelength spectrophotometric methods for simultaneous determination of binary mixtures with severely overlapping spectra

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Saleh, Sarah S.; Hassan, Nagiba Y.; Salem, Hesham

2015-02-01

This work presents the application of different spectrophotometric techniques based on two wavelengths for the determination of severely overlapped spectral components in a binary mixture without prior separation. Four novel spectrophotometric methods were developed namely: induced dual wavelength method (IDW), dual wavelength resolution technique (DWRT), advanced amplitude modulation method (AAM) and induced amplitude modulation method (IAM). The results of the novel methods were compared to that of three well-established methods which were: dual wavelength method (DW), Vierordt's method (VD) and bivariate method (BV). The developed methods were applied for the analysis of the binary mixture of hydrocortisone acetate (HCA) and fusidic acid (FSA) formulated as topical cream accompanied by the determination of methyl paraben and propyl paraben present as preservatives. The specificity of the novel methods was investigated by analyzing laboratory prepared mixtures and the combined dosage form. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed. No difference was observed between the obtained results when compared to the reported HPLC method, which proved that the developed methods could be alternative to HPLC techniques in quality control laboratories.

Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches.

PubMed

Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

2017-02-15

A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu 2+ ), cobalt ions (Co 2+ ) and nickel ions (Ni 2+ ) mixture was 0.10μgL -1 , 0.15μgL -1 and 0.13μgL -1 , respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field. Copyright © 2016 Elsevier B.V. All rights reserved.

Simultaneous determination of the brand new two-drug combination for the treatment of hepatitis C: Sofosbuvir/ledipasvir using smart spectrophotometric methods manipulating ratio spectra.

PubMed

Eissa, Maya S

2017-08-05

In this work, various sensitive and selective spectrophotometric methods were first introduced for the simultaneous determination of sofosbuvir and ledipasvir in their binary mixture without preliminary separation. Ledipasvir was determined simply by zero-order spectrophotometric method at its λ max =333.0nm in a linear range of 2.5-30.0μg/ml without any interference of sofosbuvir even in low or high concentrations and with mean percentage recovery of 100.05±0.632. Sofosbuvir can be quantitatively estimated by one of the following smart spectrophotometric methods based on ratio spectra developed for the resolution of the overlapped spectra of their binary mixture; ratio difference spectrophotometric method (RD) by computing the difference between the amplitudes of sofosbuvir ratio spectra at 228nm and 270nm, first derivative (DD 1 ) of ratio spectra by measuring the sum of amplitude of trough and peak at 265nm and 277nm, respectively, ratio subtraction (RS) spectrophotometric method in which sofosbuvir can be successfully determined at its λ max =261.0nm and mean centering (MC) of ratio spectra by measuring the mean centering values at 270nm. All of the above mentioned spectrophotometric methods can estimate sofosbuvir in a linear range of 7.5-90.0μg/ml with mean percentage recoveries of 100.57±0.810, 99.92±0.759, 99.51±0.475 and 100.75±0.672, respectively. These methods were successfully applied to the analysis of their combined dosage form and bulk powder. The adopted methods were also validated as per ICH guidelines and statistically compared to an in-house HPLC method. Copyright © 2017 Elsevier B.V. All rights reserved.

Resolution of overlapped spectra for the determination of ternary mixture using different and modified spectrophotometric methods

NASA Astrophysics Data System (ADS)

Moussa, Bahia Abbas; El-Zaher, Asmaa Ahmed; Mahrouse, Marianne Alphonse; Ahmed, Maha Said

2016-08-01

Four new spectrophotometric methods were developed, applied to resolve the overlapped spectra of a ternary mixture of [aliskiren hemifumarate (ALS)-amlodipine besylate (AM)-hydrochlorothiazide (HCT)] and to determine the three drugs in pure form and in combined dosage form. Method A depends on simultaneous determination of ALS, AM and HCT using principal component regression and partial least squares chemometric methods. In Method B, a modified isosbestic spectrophotometric method was applied for the determination of the total concentration of ALS and HCT by measuring the absorbance at 274.5 nm (isosbestic point, Aiso). On the other hand, the concentration of HCT in ternary mixture with ALS and AM could be calculated without interference using first derivative spectrophotometric method by measuring the amplitude at 279 nm (zero crossing of ALS and zero value of AM). Thus, the content of ALS was calculated by subtraction. Method C, double divisor first derivative ratio spectrophotometry (double divisor 1DD method), was based on that for the determination of one drug, the ratio spectra were obtained by dividing the absorption spectra of its different concentrations by the sum of the absorption spectra of the other two drugs as a double divisor. The first derivative of the obtained ratio spectra were then recorded using the appropriate smoothing factor. The amplitudes at 291 nm, 380 nm and 274.5 nm were selected for the determination of ALS, AM and HCT in their ternary mixture, respectively. Method D was based on mean centering of ratio spectra. The mean centered values at 287, 295.5 and 269 nm were recorded and used for the determination of ALS, AM and HCT, respectively. The developed methods were validated according to ICH guidelines and proved to be accurate, precise and selective. Satisfactory results were obtained by applying the proposed methods to the analysis of pharmaceutical dosage form.

New spectrofluorimetric and spectrophotometric methods for the determination of the analgesic drug, nalbuphine in pharmaceutical and biological fluids.

PubMed

El-Didamony, Akram M; Ali, Ismail I

2013-01-01

We describe the first studies of a simple and sensitive spectrofluorimetric and spectrophotometric methods for the analysis of nalbuphine (NLB) in dosage form and biological fluids. The spectrofluorimetric method was based on the oxidation of NLB with Ce(IV) to produce Ce(III) and its fluorescence was monitored at 352 nm after excitation at 250 nm. The spectrophotometric method involves addition of a known excess of Ce(IV) to NLB in acid medium, followed by determination of residual Ce(IV) by reacting with a fixed amount of methyl orange and measuring absorbance at 510 nm. In both methods, the amount of Ce(IV) reacted corresponds to the amount of NLB and measured fluorescence or absorbance were found to increase linearly with the concentration of NLB, which are corroborated by correlation coefficients of 0.9997 and 0.9999 for spectrofluorimetric and spectrophotometric methods, respectively. Different variables affecting the reaction conditions such as concentrations of Ce(IV), type and concentration of acid medium, reaction time, temperature, and diluting solvents were carefully studied and optimized. The accuracy and precision of the methods were evaluated on intra-day and inter-day basis. The proposed methods were successfully applied for the determination of NLB in pharmaceutical formulation and biological samples with good recoveries. Copyright © 2012 John Wiley & Sons, Ltd.

Analysis of ultraviolet spectrophotometric data from Copernicus

NASA Technical Reports Server (NTRS)

Snow, T. P., Jr.

1979-01-01

Ultraviolet spectral data from the OAO 3 satellite are being used to study interstellar absorption lines and stellar and circumstellar lines in hot stars. The interstellar data are beneficial in analyzing the depletions of heavy elements from the gas phase and in elucidating how these depletions depend on physical conditions. Abundances in separate velocity components were determined from line profiles. Observations were carried out for interstellar abundances, both atomic and molecular, towards a number of stars. The better quality data are being analyzed for profile information and the lesser data are being used in curve-of-growth analyses. Molecular observations were carried out as well, N2 was sought; interstellar C2 was detected and its rotational excitation utilized to establish limits in interstellar cloud temperatures. An extensive search for H2O resulted in a tentative identification which will produce new information on chemical reaction rates. Interstellar depletions and grain properties in the rho Ophiuchi cloud, stellar wind variability, and circumstellar lines are also under study.

Spectroflourometric and spectrophotometric methods for the determination of sitagliptin in binary mixture with metformin and ternary mixture with metformin and sitagliptin alkaline degradation product.

PubMed

El-Bagary, Ramzia I; Elkady, Ehab F; Ayoub, Bassam M

2011-03-01

Simple, accurate and precise spectroflourometric and spectrophotometric methods have been developed and validated for the determination of sitagliptin phosphate monohydrate (STG) and metformin HCL (MET). Zero order, first derivative, ratio derivative spectrophotometric methods and flourometric methods have been developed. The zero order spectrophotometric method was used for the determination of STG in the range of 50-300 μg mL(-1). The first derivative spectrophotometric method was used for the determination of MET in the range of 2-12 μg mL(-1) and STG in the range of 50-300 μg mL(-1) by measuring the peak amplitude at 246.5 nm and 275 nm, respectively. The first derivative of ratio spectra spectrophotometric method used the peak amplitudes at 232 nm and 239 nm for the determination of MET in the range of 2-12 μg mL(-1). The flourometric method was used for the determination of STG in the range of 0.25-110 μg mL(-1). The proposed methods used to determine each drug in binary mixture with metformin and ternary mixture with metformin and sitagliptin alkaline degradation product that is obtained after alkaline hydrolysis of sitagliptin. The results were statistically compared using one-way analysis of variance (ANOVA). The methods developed were satisfactorily applied to the analysis of the pharmaceutical formulations and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

Spectroflourometric and Spectrophotometric Methods for the Determination of Sitagliptin in Binary Mixture with Metformin and Ternary Mixture with Metformin and Sitagliptin Alkaline Degradation Product

PubMed Central

El-Bagary, Ramzia I.; Elkady, Ehab F.; Ayoub, Bassam M.

2011-01-01

Simple, accurate and precise spectroflourometric and spectrophotometric methods have been developed and validated for the determination of sitagliptin phosphate monohydrate (STG) and metformin HCL (MET). Zero order, first derivative, ratio derivative spectrophotometric methods and flourometric methods have been developed. The zero order spectrophotometric method was used for the determination of STG in the range of 50-300 μg mL-1. The first derivative spectrophotometric method was used for the determination of MET in the range of 2–12 μg mL-1 and STG in the range of 50-300 μg mL-1 by measuring the peak amplitude at 246.5 nm and 275 nm, respectively. The first derivative of ratio spectra spectrophotometric method used the peak amplitudes at 232 nm and 239 nm for the determination of MET in the range of 2–12 μg mL-1. The flourometric method was used for the determination of STG in the range of 0.25-110 μg mL-1. The proposed methods used to determine each drug in binary mixture with metformin and ternary mixture with metformin and sitagliptin alkaline degradation product that is obtained after alkaline hydrolysis of sitagliptin. The results were statistically compared using one-way analysis of variance (ANOVA). The methods developed were satisfactorily applied to the analysis of the pharmaceutical formulations and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms. PMID:23675222

Optimized and Validated Spectrophotometric Methods for the Determination of Enalapril Maleate in Commercial Dosage Forms

PubMed Central

Rahman, Nafisur; Haque, Sk Manirul

2008-01-01

Four simple, rapid and sensitive spectrophotometric methods have been proposed for the determination of enalapril maleate in pharmaceutical formulations. The first method is based on the reaction of carboxylic acid group of enalapril maleate with a mixture of potassium iodate (KIO3) and iodide (KI) to form yellow colored product in aqueous medium at 25 ± 1°C. The reaction is followed spectrophotometrically by measuring the absorbance at 352 nm. The second, third and fourth methods are based on the charge transfer complexation reaction of the drug with p-chloranilic acid (pCA) in 1, 4-dioxan-methanol medium, 2, 3-dichloro 5, 6-dicyano 1, 4-benzoquinone (DDQ) in acetonitrile-1,4 dioxane medium and iodine in acetonitrile-dichloromethane medium. Under optimized experimental conditions, Beer’s law is obeyed in the concentration ranges of 2.5–50, 20–560, 5–75 and 10–200 μg mL−1, respectively. All the methods have been applied to the determination of enalapril maleate in pharmaceutical dosage forms. Results of analysis are validated statistically. PMID:19609388

Method for removal of phosgene from boron trichloride

DOEpatents

Freund, S.M.

1983-09-20

Selective ultraviolet photolysis using an unfiltered mercury arc lamp has been used to substantially reduce the phosgene impurity in a mixture of boron trichloride and phosgene. Infrared spectrophotometric analysis of the sample before and after irradiation shows that it is possible to highly purify commercially available boron trichloride with this method. 5 figs.

Is it possible to screen for milk or whey protein adulteration with melamine, urea and ammonium sulphate, combining Kjeldahl and classical spectrophotometric methods?

PubMed

Finete, Virgínia de Lourdes Mendes; Gouvêa, Marcos Martins; Marques, Flávia Ferreira de Carvalho; Netto, Annibal Duarte Pereira

2013-12-15

The Kjeldahl method and four classic spectrophotometric methods (Biuret, Lowry, Bradford and Markwell) were applied to evaluate the protein content of samples of UHT whole milk deliberately adulterated with melamine, ammonium sulphate or urea, which can be used to defraud milk protein and whey contents. Compared with the Kjeldahl method, the response of the spectrophotometric methods was unaffected by the addition of the nitrogen compounds to milk or whey. The methods of Bradford and Markwell were most robust and did not exhibit interference subject to composition. However, the simultaneous interpretation of results obtained using these methods with those obtained using the Kjeldahl method indicated the addition of nitrogen-rich compounds to milk and/or whey. Therefore, this work suggests a combination of results of Kjeldahl and spectrophotometric methods should be used to screen for milk adulteration by these compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

The effect of suspended sediment and color on ultraviolet spectrophotometric nitrate sensors

USGS Publications Warehouse

Snazelle, Teri T.

2016-03-08

Four commercially available ultraviolet nitrate spectrophotometric sensors were evaluated by the U.S. Geological Survey Hydrologic Instrumentation Facility (HIF) to determine the effects of suspended sediment concentration (SSC) and colored dissolved organic matter (CDOM) on sensor accuracy. The evaluated sensors were: the Hach NITRATAX plus sc (5-millimeters (mm) path length), Hach NITRATAX plus sc (2 mm), S::CAN Spectro::lyser (5 mm), and the Satlantic SUNA V2 (5 mm). A National Institute of Standards and Technology-traceable nitrate-free sediment standard was purchased and used to create the turbid environment, and an easily made filtered tea solution was used for the CDOM test. All four sensors performed well in the test that evaluated the effect of suspended sediment on accuracy. The Hach 5 mm, Hach 2 mm, and the SUNA V2 met their respective manufacturer accuracy specifications up to concentrations of 4,500 milligrams per liter (mg/L) SSC. The S::CAN failed to meet its accuracy specifications when the SSC concentrations exceeded 4,000 mg/L. Test results from the effect of CDOM on accuracy indicated a significant skewing of data from all four sensors and showed an artificial elevation of measured nitrate to varying amounts. Of the four sensors tested, the Satlantic SUNA V2’s accuracy was affected the least in the CDOM test. The nitrate concentration measured by the SUNA V2 was approximately 24 percent higher than the actual concentration when estimated total organic carbon values exceeded 44 mg/L. Measured nitrate concentration falsely increased 49 percent when measured by the Hach 5 mm, and 75 percent when measured by the Hach 2 mm. The S::CAN’s reported nitrate concentration increased 96 percent. Path length plays an important role in the sensor’s ability to compensate measurements for matrix interferences, but does not solely determine how well a sensor can handle all interferences. The sensor’s proprietary algorithms also play a key role in matrix

Comparative study of novel versus conventional two-wavelength spectrophotometric methods for analysis of spectrally overlapping binary mixture.

PubMed

Lotfy, Hayam M; Hegazy, Maha A; Rezk, Mamdouh R; Omran, Yasmin Rostom

2015-09-05

Smart spectrophotometric methods have been applied and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and prednisolone acetate (PA) without preliminary separation. Two novel methods have been developed; the first method depends upon advanced absorbance subtraction (AAS), while the other method relies on advanced amplitude modulation (AAM); in addition to the well established dual wavelength (DW), ratio difference (RD) and constant center coupled with spectrum subtraction (CC-SS) methods. Accuracy, precision and linearity ranges of these methods were determined. Moreover, selectivity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied to the assay of drugs in their pharmaceutical formulations. No interference was observed from common additives and the validity of the methods was tested. The obtained results have been statistically compared to that of official spectrophotometric methods to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel Spectrophotometric Method for the Assay of Captopril in Dosage Forms using 2,6-Dichloroquinone-4-Chlorimide

PubMed Central

El-Enany, Nahed; Belal, Fathalla; Rizk, Mohamed

2008-01-01

A simple spectrophotometric method was developed for the determination of captopril (CPL) in pharmaceutical preparations. The method is based on coupling captopril with 2,6-dichloroquinone-4-chlorimide (DCQ) in dimethylsulphoxide. The yellow reaction product was measured at 443 nm. The absorbance–concentration plot was rectilinear over the range of 10-50 μg/mL with minimum detection limit (LOD) of 0.66 μg/mL and a quantification limit (LOQ) of 2.0 μg/mL. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The proposed method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained using official and reference spectrophotometric methods. Hydrochlorothiazide which is frequently co-formulated with CPL did not interfere with the assay. A proposal of the reaction pathway was presented. PMID:23675082

Simple, fast and reliable liquid chromatographic and spectrophotometric methods for the determination of theophylline in urine, saliva and plasma samples.

PubMed

Charehsaz, Mohammad; Gürbay, Aylin; Aydin, Ahmet; Sahin, Gönül

2014-01-01

In this study, a high-performance liquid chromatographic method (HPLC) and UV spectrophotometric method were developed, validated and applied for the determination of theophylline in biological fluids. Liquid- liquid extraction is performed for isolation of the drug and elimination of plasma and saliva interferences. Urine samples were applied without any extraction. The chromatographic separation was achieved on a C18 column by using 60:40 methanol:water as mobile phase under isocratic conditions at a flow rate of 0.75 mL/min with UV detection at 280 nm in HPLC method. UV spectrophotometric analysis was performed at 275 nm. the limit of quantification: 1.1 µg/mL for urine, 1.9 µg/mL for saliva, 3.1 µg/mL for plasma; recovery: 94.85% for plasma, 100.45% for saliva, 101.39% for urine; intra-day precision: 0.22-2.33%, inter-day precision: 3.17-13.12%. Spectrophotometric analysis results were as follows: the limit of quantitation: 5.23 µg/mL for plasma, 8.7 µg/mL for urine; recovery: 98.27% for plasma, 95.25% for urine; intra-day precision: 2.37 - 3.00%, inter-day precision: 5.43-7.91%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of theophylline in biological samples. Also spectrophotometric analysis can be used where it can be applicable.

Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form.

PubMed

Mendez, Andreas S L; Steppe, Martin; Schapoval, Elfrides E S

2003-12-04

A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 degrees C was studied. The results were satisfactory with good stability after 24 h at 4 degrees C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.

Evaluation of spectrophotometric and HPLC methods for shikimic acid determination in plants: models in glyphosate-resistant and -susceptible crops.

PubMed

Zelaya, Ian A; Anderson, Jennifer A H; Owen, Micheal D K; Landes, Reid D

2011-03-23

Endogenous shikimic acid determinations are routinely used to assess the efficacy of glyphosate in plants. Numerous analytical methods exist in the public domain for the detection of shikimic acid, yet the most commonly cited comprise spectrophotometric and high-pressure liquid chromatography (HPLC) methods. This paper compares an HPLC and two spectrophotometric methods (Spec 1 and Spec 2) and assesses the effectiveness in the detection of shikimic acid in the tissues of glyphosate-treated plants. Furthermore, the study evaluates the versatility of two acid-based shikimic acid extraction methods and assesses the longevity of plant extract samples under different storage conditions. Finally, Spec 1 and Spec 2 are further characterized with respect to (1) the capacity to discern between shikimic acid and chemically related alicyclic hydroxy acids, (2) the stability of the chromophore (t1/2), (3) the detection limits, and (4) the cost and simplicity of undertaking the analytical procedure. Overall, spectrophotometric methods were more cost-effective and simpler to execute yet provided a narrower detection limit compared to HPLC. All three methods were specific to shikimic acid and detected the compound in the tissues of glyphosate-susceptible crops, increasing exponentially in concentration within 24 h of glyphosate application and plateauing at approximately 72 h. Spec 1 estimated more shikimic acid in identical plant extract samples compared to Spec 2 and, likewise, HPLC detection was more effective than spectrophotometric determinations. Given the unprecedented global adoption of glyphosate-resistant crops and concomitant use of glyphosate, an effective and accurate assessment of glyphosate efficacy is important. Endogenous shikimic acid determinations are instrumental in corroborating the efficacy of glyphosate and therefore have numerous applications in herbicide research and related areas of science as well as resolving many commercial issues as a consequence of

A comparative study of smart spectrophotometric methods for simultaneous determination of a skeletal muscle relaxant and an analgesic in combined dosage form.

PubMed

Salem, Hesham; Mohamed, Dalia

2015-04-05

Six simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the analgesic drug; paracetamol (PARA) and the skeletal muscle relaxant; dantrolene sodium (DANT). Three methods are manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and mean centering (MC). The other three methods are utilizing the isoabsorptive point either at zero order namely; absorbance ratio (AR) and absorbance subtraction (AS) or at ratio spectrum namely; amplitude modulation (AM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined dosage form. Standard deviation values are less than 1.5 in the assay of raw materials and capsules. The obtained results were statistically compared with each other and with those of reported spectrophotometric ones. The comparison showed that there is no significant difference between the proposed methods and the reported methods regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

A comparative study of smart spectrophotometric methods for simultaneous determination of a skeletal muscle relaxant and an analgesic in combined dosage form

NASA Astrophysics Data System (ADS)

Salem, Hesham; Mohamed, Dalia

2015-04-01

Six simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the analgesic drug; paracetamol (PARA) and the skeletal muscle relaxant; dantrolene sodium (DANT). Three methods are manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and mean centering (MC). The other three methods are utilizing the isoabsorptive point either at zero order namely; absorbance ratio (AR) and absorbance subtraction (AS) or at ratio spectrum namely; amplitude modulation (AM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined dosage form. Standard deviation values are less than 1.5 in the assay of raw materials and capsules. The obtained results were statistically compared with each other and with those of reported spectrophotometric ones. The comparison showed that there is no significant difference between the proposed methods and the reported methods regarding both accuracy and precision.

Validated derivative and ratio derivative spectrophotometric methods for the simultaneous determination of levocetirizine dihydrochloride and ambroxol hydrochloride in pharmaceutical dosage form

NASA Astrophysics Data System (ADS)

Ali, Omnia I. M.; Ismail, Nahla S.; Elgohary, Rasha M.

2016-01-01

Three simple, precise, accurate and validated derivative spectrophotometric methods have been developed for the simultaneous determination of levocetirizine dihydrochloride (LCD) and ambroxol hydrochloride (ABH) in bulk powder and in pharmaceutical formulations. The first method is a first derivative spectrophotometric method (1D) using a zero-crossing technique of measurement at 210.4 nm for LCD and at 220.0 nm for ABH. The second method employs a second derivative spectrophotometry (2D) where the measurements were carried out at 242.0 and 224.4 nm for LCD and ABH, respectively. In the third method, the first derivative of the ratio spectra was calculated and the first derivative of the ratio amplitudes at 222.8 and 247.2 nm was selected for the determination of LCD and ABH, respectively. Calibration graphs were established in the ranges of 1.0-20.0 μg mL- 1 for LCD and 4.0-20.0 μg mL- 1 for ABH using derivative and ratio first derivative spectrophotometric methods with good correlation coefficients. The developed methods have been successfully applied to the simultaneous determination of both drugs in commercial tablet dosage form.

Validated derivative and ratio derivative spectrophotometric methods for the simultaneous determination of levocetirizine dihydrochloride and ambroxol hydrochloride in pharmaceutical dosage form.

PubMed

Ali, Omnia I M; Ismail, Nahla S; Elgohary, Rasha M

2016-01-15

Three simple, precise, accurate and validated derivative spectrophotometric methods have been developed for the simultaneous determination of levocetirizine dihydrochloride (LCD) and ambroxol hydrochloride (ABH) in bulk powder and in pharmaceutical formulations. The first method is a first derivative spectrophotometric method ((1)D) using a zero-crossing technique of measurement at 210.4 nm for LCD and at 220.0 nm for ABH. The second method employs a second derivative spectrophotometry ((2)D) where the measurements were carried out at 242.0 and 224.4 nm for LCD and ABH, respectively. In the third method, the first derivative of the ratio spectra was calculated and the first derivative of the ratio amplitudes at 222.8 and 247.2 nm was selected for the determination of LCD and ABH, respectively. Calibration graphs were established in the ranges of 1.0-20.0 μg mL(-1) for LCD and 4.0-20.0 μg mL(-1) for ABH using derivative and ratio first derivative spectrophotometric methods with good correlation coefficients. The developed methods have been successfully applied to the simultaneous determination of both drugs in commercial tablet dosage form. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and Characterization of Potassium Tris(oxalato)ferrate(III) Trihydrate: A Spectrophotometric Method of Iron Analysis

NASA Astrophysics Data System (ADS)

Dallinger, Richard F.

1995-10-01

A previous Journal article [J. Chem. Educ. 1984, 61, 1098--1099] described a potassium tris(oxalato)ferrate(III) trihydrate empirical formula experiment that offered an excellent integrative experience in synthesis and characterization for general chemistry laboratory students. However, we have introduced a fast and accurate spectrophotometric method for the determination of iron in the product that takes the place of the photochemical-gravimetric procedure described in the article. Besides the pedagogic interest of bringing three different types of chemical analysis (titrimetric, gravimetric, and spectrophotometric) to bear on one compound, the new iron determination allows students to complete the experiment in 2, 3-hr laboratory periods rather than the 5 periods allotted in the original experiment.

From thermometric to spectrophotometric kinetic-catalytic methods of analysis. A review.

PubMed

Cerdà, Víctor; González, Alba; Danchana, Kaewta

2017-05-15

Kinetic-catalytic analytical methods have proved to be very easy and highly sensitive strategies for chemical analysis, that rely on simple instrumentation [1,2]. Molecular absorption spectrophotometry is commonly used as the detection technique. However, other detection systems, like electrochemical or thermometric ones, offer some interesting possibilities since they are not affected by the color or turbidity of the samples. In this review some initial experience with thermometric kinetic-catalytic methods is described, up to our current experience exploiting spectrophotometric flow techniques to automate this kind of reactions, including the use of integrated chips. Procedures for determination of inorganic and organic species in organic and inorganic matrices are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

Resolution of overlapped spectra for the determination of ternary mixture using different and modified spectrophotometric methods.

PubMed

Moussa, Bahia Abbas; El-Zaher, Asmaa Ahmed; Mahrouse, Marianne Alphonse; Ahmed, Maha Said

2016-08-05

Four new spectrophotometric methods were developed, applied to resolve the overlapped spectra of a ternary mixture of [aliskiren hemifumarate (ALS)-amlodipine besylate (AM)-hydrochlorothiazide (HCT)] and to determine the three drugs in pure form and in combined dosage form. Method A depends on simultaneous determination of ALS, AM and HCT using principal component regression and partial least squares chemometric methods. In Method B, a modified isosbestic spectrophotometric method was applied for the determination of the total concentration of ALS and HCT by measuring the absorbance at 274.5nm (isosbestic point, Aiso). On the other hand, the concentration of HCT in ternary mixture with ALS and AM could be calculated without interference using first derivative spectrophotometric method by measuring the amplitude at 279nm (zero crossing of ALS and zero value of AM). Thus, the content of ALS was calculated by subtraction. Method C, double divisor first derivative ratio spectrophotometry (double divisor (1)DD method), was based on that for the determination of one drug, the ratio spectra were obtained by dividing the absorption spectra of its different concentrations by the sum of the absorption spectra of the other two drugs as a double divisor. The first derivative of the obtained ratio spectra were then recorded using the appropriate smoothing factor. The amplitudes at 291nm, 380nm and 274.5nm were selected for the determination of ALS, AM and HCT in their ternary mixture, respectively. Method D was based on mean centering of ratio spectra. The mean centered values at 287, 295.5 and 269nm were recorded and used for the determination of ALS, AM and HCT, respectively. The developed methods were validated according to ICH guidelines and proved to be accurate, precise and selective. Satisfactory results were obtained by applying the proposed methods to the analysis of pharmaceutical dosage form. Copyright © 2016. Published by Elsevier B.V.

Verification of spectrophotometric method for nitrate analysis in water samples

NASA Astrophysics Data System (ADS)

Kurniawati, Puji; Gusrianti, Reny; Dwisiwi, Bledug Bernanti; Purbaningtias, Tri Esti; Wiyantoko, Bayu

2017-12-01

The aim of this research was to verify the spectrophotometric method to analyze nitrate in water samples using APHA 2012 Section 4500 NO3-B method. The verification parameters used were: linearity, method detection limit, level of quantitation, level of linearity, accuracy and precision. Linearity was obtained by using 0 to 50 mg/L nitrate standard solution and the correlation coefficient of standard calibration linear regression equation was 0.9981. The method detection limit (MDL) was defined as 0,1294 mg/L and limit of quantitation (LOQ) was 0,4117 mg/L. The result of a level of linearity (LOL) was 50 mg/L and nitrate concentration 10 to 50 mg/L was linear with a level of confidence was 99%. The accuracy was determined through recovery value was 109.1907%. The precision value was observed using % relative standard deviation (%RSD) from repeatability and its result was 1.0886%. The tested performance criteria showed that the methodology was verified under the laboratory conditions.

Spectrophotometric methods as a novel screening approach for analysis of dihydropyrimidine dehydrogenase activity before treatment with 5-fluorouracil chemotherapy.

PubMed

Dolegowska, B; Ostapowicz, A; Stanczyk-Dunaj, M; Blogowski, W

2012-08-01

5-Fluorouracil (5-FU) is one of the most commonly used chemotherapeutics in the treatment of malignancies originating from breast, prostate, ovarian, skin and gastrointestinal tissues. Around 80% of administered dose of 5-FU is catabolized by dihydropirymidine dehydrogenase (DPD). Patients, in whom a deficiency or insufficient activity of this enzyme is observed, are at great risk of development of severe, even lethal, 5-FU toxicity. According to recent studies, so far over 30 mutations of DPYD gene, which are associated with DPD deficiency/insufficiency, have already been discovered. Currently, there are several analytical methods used for measurements of DPD activity. However, in this paper we report a novel, simple, economical and more accessible spectrophotometric method for measurements of DPD activity in the peripheral blood mononuclear cells (PBMCs) that was developed and validated on analysis of 200 generally healthy volunteers aged 22-63. We present two spectrophotometric protocols in this study, and as a reference method we used already described reverse phase high-performance liquid chromatography (RP HPLC) analysis. Basing on our findings, we conclude that spectrophotometric methods may be used as a screening protocol preceding 5-FU-based chemotherapy. Nevertheless, before introduction into clinical reality, our results should be confirmed in further larger studies.

A review of ultraviolet astronomical research with the Copernicus satellite

NASA Technical Reports Server (NTRS)

Snow, T. P., Jr.

1976-01-01

Results of ultraviolet spectrophotometric observations with the satellite Copernicus (OAO-3) are summarized, and are intended to be completely covered through January 1, 1976. Interstellar research recently reviewed elsewhere is not included, although some newer interstellar results are described. A large fraction of the research covered in this review has been carried out by Guest Investigators with Copernicus. A brief description of the spacecraft and its operation is included.

Spectrophotometric method for the determination of paraquat in water, grain and plant materials.

PubMed

Shivhare, P; Gupta, V K

1991-04-01

A sensitive spectrophotometric method for the determination of paraquat using ascorbic acid (an easily available reducing agent) is described. Paraquat is reduced with ascorbic acid in alkaline solution to give a blue radical ion with an absorbance maximum at 600 nm. Beer's law is obeyed in the range 12-96 micrograms of paraquat in 10 ml of the final solution (1.2-9.6 ppm). The important analytical parameters and the optimum reaction conditions were evaluated. The method was applied successfully to the determination of paraquat in water, grain and plant materials.

New potentiometric and spectrophotometric methods for the determination of dextromethorphan in pharmaceutical preparations.

PubMed

Elmosallamy, Mohamed A F; Amin, Alaa S

2014-01-01

New, simple and convenient potentiometric and spectrophotometric methods are described for the determination of dextromethorphan hydrobromide (DXM) in pharmaceutical preparations. The potentiometric technique is based on developing a potentiometric sensor incorporating the dextromethorphan tetrakis(p-chlorophenyl)borate ion-pair complex as an electroactive species in a plasticized PVC matrix membrane with o-nitophenyl octyl ether or dioctyl phthalate. The sensor shows a rapid near Nernstian response of over 1 × 10(-5) - 1 × 10(-2) mol L(-1) dextromethorphan in the pH range of 3.0 - 9.0. The detection limit is 2 × 10(-6) mol L(-1) DXM and the response time is instantaneous (2 s). The proposed spectrophotometric technique involves the reaction of DXM with eriochrom black T (EBT) to form an ion-associate complex. Solvent extraction is used to improve the selectivity of the method. The optimal extraction and reaction conditions have been studied, and the analytical characteristics of the method have been obtained. Linearity is obeyed in the range of 7.37 - 73.7 × 10(-5) mol L(-1) DXM, and the detection limit of the method is 1.29 × 10(-5) mol L(-1). The relative standard deviation (RSD) and relative error for six replicate measurements of 3.685 × 10(-4) mol L(-1) are 0.672 and 0.855%, respectively. The interference effect of some excepients has also been tested. The drug contents in pharmaceutical preparations were successfully determined by the proposed methods by applying the standard-addition technique.

Spectrophotometric and spectrofluorimetric methods for determination of certain biologically active phenolic drugs in their bulk powders and different pharmaceutical formulations.

PubMed

Omar, Mahmoud A; Badr El-Din, Kalid M; Salem, Hesham; Abdelmageed, Osama H

2018-03-05

Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354nm (λ excitation =255nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0μgmL -1 , 20.0-24.0ngmL -1 with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624μgmL -1 respectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74ngmL -1 respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods showed

Spectrophotometric and spectrofluorimetric methods for determination of certain biologically active phenolic drugs in their bulk powders and different pharmaceutical formulations

NASA Astrophysics Data System (ADS)

Omar, Mahmoud A.; Badr El-Din, Kalid M.; Salem, Hesham; Abdelmageed, Osama H.

2018-03-01

Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317 nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354 nm (λexcitation = 255 nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0 μg mL- 1, 20.0-24.0 ng mL- 1 with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624 μg mL- 1respectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74 ng mL- 1 respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods

Validated spectrophotometric methods for determination of sodium valproate based on charge transfer complexation reactions.

PubMed

Belal, Tarek S; El-Kafrawy, Dina S; Mahrous, Mohamed S; Abdel-Khalek, Magdi M; Abo-Gharam, Amira H

2016-02-15

This work presents the development, validation and application of four simple and direct spectrophotometric methods for determination of sodium valproate (VP) through charge transfer complexation reactions. The first method is based on the reaction of the drug with p-chloranilic acid (p-CA) in acetone to give a purple colored product with maximum absorbance at 524nm. The second method depends on the reaction of VP with dichlone (DC) in dimethylformamide forming a reddish orange product measured at 490nm. The third method is based upon the interaction of VP and picric acid (PA) in chloroform resulting in the formation of a yellow complex measured at 415nm. The fourth method involves the formation of a yellow complex peaking at 361nm upon the reaction of the drug with iodine in chloroform. Experimental conditions affecting the color development were studied and optimized. Stoichiometry of the reactions was determined. The proposed spectrophotometric procedures were effectively validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curves of the formed color products with p-CA, DC, PA and iodine showed good linear relationships over the concentration ranges 24-144, 40-200, 2-20 and 1-8μg/mL respectively. The proposed methods were successfully applied to the assay of sodium valproate in tablets and oral solution dosage forms with good accuracy and precision. Assay results were statistically compared to a reference pharmacopoeial HPLC method where no significant differences were observed between the proposed methods and reference method. Copyright © 2015 Elsevier B.V. All rights reserved.

Validated spectrophotometric methods for determination of sodium valproate based on charge transfer complexation reactions

NASA Astrophysics Data System (ADS)

Belal, Tarek S.; El-Kafrawy, Dina S.; Mahrous, Mohamed S.; Abdel-Khalek, Magdi M.; Abo-Gharam, Amira H.

2016-02-01

This work presents the development, validation and application of four simple and direct spectrophotometric methods for determination of sodium valproate (VP) through charge transfer complexation reactions. The first method is based on the reaction of the drug with p-chloranilic acid (p-CA) in acetone to give a purple colored product with maximum absorbance at 524 nm. The second method depends on the reaction of VP with dichlone (DC) in dimethylformamide forming a reddish orange product measured at 490 nm. The third method is based upon the interaction of VP and picric acid (PA) in chloroform resulting in the formation of a yellow complex measured at 415 nm. The fourth method involves the formation of a yellow complex peaking at 361 nm upon the reaction of the drug with iodine in chloroform. Experimental conditions affecting the color development were studied and optimized. Stoichiometry of the reactions was determined. The proposed spectrophotometric procedures were effectively validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curves of the formed color products with p-CA, DC, PA and iodine showed good linear relationships over the concentration ranges 24-144, 40-200, 2-20 and 1-8 μg/mL respectively. The proposed methods were successfully applied to the assay of sodium valproate in tablets and oral solution dosage forms with good accuracy and precision. Assay results were statistically compared to a reference pharmacopoeial HPLC method where no significant differences were observed between the proposed methods and reference method.

Titrimetric and Spectrophotometric Methods for the Assay of Ketotifen Using Cerium(IV) and Two Reagents

PubMed Central

Raghu, Madihalli Srinivas; Basavaiah, Kanakapura; Prashanth, Kudige Nagaraj; Vinay, Kanakapura Basavaiah

2013-01-01

One titrimetric and two spectrophotometric methods are described for the determination of ketotifen fumarate (KTF) in bulk drug and in tablets using cerium(IV) as the oxidimetric agent. In titrimetry (method A), the drug was treated with a measured excess of cerium(IV) in H2SO4 medium and after a standing time of 10 min, the surplus oxidant was determined by back titration with iron(II). The spectrophotometric procedures involve addition of a known excess of cerium(IV) to KTF in acid medium followed by the determination of unreacted oxidant by reacting with either p-dimethyl amino benzaldehyde and measuring the resulting colour at 460 nm (method B) or o-dianisidine and subsequent measurement of the absorbance of coloured product at 470 nm (method C). Titrimetric assay is based on a 1 : 2 reaction stoichiometry between KTF and cerium(IV) and the method is applicable over 2–18 mg range. In spectrophotometry, regression analysis of Beer's law plots showed a good correlation in 0.4–8.0 and 0.4–10.0 g mL−1 KTF ranges for method B and method C, respectively, and the corresponding molar absorptivity coefficients are calculated to be 4.0 × 104 and 3.7 × 104 L mol−1 cm−1. PMID:24324496

Optimization of a direct spectrophotometric method to investigate the kinetics and inhibition of sialidases

PubMed Central

2012-01-01

Backgrounds Streptococcus pneumoniae expresses three distinct sialidases, NanA, NanB, and NanC, that are believed to be key virulence factors and thus, potential important drug targets. We previously reported that the three enzymes release different products from sialosides, but could share a common catalytic mechanism before the final step of product formation. However, the kinetic investigations of the three sialidases have not been systematically done thus far, due to the lack of an easy and steady measurement of sialidase reaction rate. Results In this work, we present further kinetic characterization of pneumococcal sialidases by using a direct spectrophotometric method with the chromogenic substrate p-nitrophenyl-N-acetylneuraminic acid (p-NP-Neu5Ac). Using our assay, the measured kinetic parameters of the three purified pneumococcal sialidase, NanA, NanB and NanC, were obtained and were in perfect agreement with the previously published data. The major advantage of this alternative method resides in the direct measurement of the released product, allowing to readily determine of initial reaction rates and record complete hydrolysis time courses. Conclusion We developed an accurate, fast and sensitive spectrophotometric method to investigate the kinetics of sialidase-catalyzed reactions. This fast, sensitive, inexpensive and accurate method could benefit the study of the kinetics and inhibition of sialidases in general. PMID:23031230

Development of microwave assisted spectrophotometric method for the determination of glucose

NASA Astrophysics Data System (ADS)

Ali, Asif; Hussain, Zahid; Arain, Muhammad Balal; Shah, Nasrullah; Khan, Khalid Mohammad; Gulab, Hussain; Zada, Amir

2016-01-01

A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL- 1 and 9.33 μg mL- 1 with standard deviation of ± 0.05. The developed method was also applicable to urine sample.

A comparative study of smart spectrophotometric methods for simultaneous determination of sitagliptin phosphate and metformin hydrochloride in their binary mixture.

PubMed

Lotfy, Hayam M; Mohamed, Dalia; Mowaka, Shereen

2015-01-01

Simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the oral antidiabetic drugs; sitagliptin phosphate (STG) and metformin hydrochloride (MET) in combined pharmaceutical formulations. Three methods were manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and a novel approach of induced amplitude modulation (IAM) methods. The first two methods were used for determination of STG, while MET was directly determined by measuring its absorbance at λmax 232 nm. However, (IAM) was used for the simultaneous determination of both drugs. Moreover, another three methods were developed based on derivative spectroscopy followed by mathematical manipulation steps namely; amplitude factor (P-factor), amplitude subtraction (AS) and modified amplitude subtraction (MAS). In addition, in this work the novel sample enrichment technique named spectrum addition was adopted. The proposed spectrophotometric methods did not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined pharmaceutical formulations. Standard deviation values were less than 1.5 in the assay of raw materials and tablets. The obtained results were statistically compared to that of a reported spectrophotometric method. The statistical comparison showed that there was no significant difference between the proposed methods and the reported one regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Two smart spectrophotometric methods for the simultaneous estimation of Simvastatin and Ezetimibe in combined dosage form

NASA Astrophysics Data System (ADS)

Magdy, Nancy; Ayad, Miriam F.

2015-02-01

Two simple, accurate, precise, sensitive and economic spectrophotometric methods were developed for the simultaneous determination of Simvastatin and Ezetimibe in fixed dose combination products without prior separation. The first method depends on a new chemometrics-assisted ratio spectra derivative method using moving window polynomial least square fitting method (Savitzky-Golay filters). The second method is based on a simple modification for the ratio subtraction method. The suggested methods were validated according to USP guidelines and can be applied for routine quality control testing.

An ultraviolet-visible spectrophotometer automation system. Part 3: Program documentation

NASA Astrophysics Data System (ADS)

Roth, G. S.; Teuschler, J. M.; Budde, W. L.

1982-07-01

The Ultraviolet-Visible Spectrophotometer (UVVIS) automation system accomplishes 'on-line' spectrophotometric quality assurance determinations, report generations, plot generations and data reduction for chlorophyll or color analysis. This system also has the capability to process manually entered data for the analysis of chlorophyll or color. For each program of the UVVIS system, this document contains a program description, flowchart, variable dictionary, code listing, and symbol cross-reference table. Also included are descriptions of file structures and of routines common to all automated analyses. The programs are written in Data General extended BASIC, Revision 4.3, under the RDOS operating systems, Revision 6.2. The BASIC code has been enhanced for real-time data acquisition, which is accomplished by CALLS to assembly language subroutines. Two other related publications are 'An Ultraviolet-Visible Spectrophotometer Automation System - Part I Functional Specifications,' and 'An Ultraviolet-Visible Spectrophotometer Automation System - Part II User's Guide.'

Validation of four different spectrophotometric methods for simultaneous determination of Domperidone and Ranitidine in bulk and pharmaceutical formulation.

PubMed

Abdel-Ghany, Maha F; Abdel-Aziz, Omar; Mohammed, Yomna Y

2015-01-01

Four simple, specific, accurate and precise spectrophotometric methods were developed and validated for simultaneous determination of Domperidone (DP) and Ranitidine Hydrochloride (RT) in bulk powder and pharmaceutical formulation. The first method was simultaneous ratio subtraction (SRS), the second was ratio subtraction (RS) coupled with zero order spectrophotometry (D(0)), the third was first derivative of the ratio spectra ((1)DD) and the fourth method was mean centering of ratio spectra (MCR). The calibration curve is linear over the concentration range of 0.5-5 and 1-45 μg mL(-1) for DP and RT, respectively. The proposed spectrophotometric methods can analyze both drugs without any prior separation steps. The selectivity of the adopted methods was tested by analyzing synthetic mixtures of the investigated drugs, also in their pharmaceutical formulation. The suggested methods were validated according to International Conference of Harmonization (ICH) guidelines and the results revealed that; they were precise and reproducible. All the obtained results were statistically compared with those of the reported method, where there was no significant difference. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and Validation of Chemometric Spectrophotometric Methods for Simultaneous Determination of Simvastatin and Nicotinic Acid in Binary Combinations.

PubMed

Alahmad, Shoeb; Elfatatry, Hamed M; Mabrouk, Mokhtar M; Hammad, Sherin F; Mansour, Fotouh R

2018-01-01

The development and introduction of combined therapy represent a challenge for analysis due to severe overlapping of their UV spectra in case of spectroscopy or the requirement of a long tedious and high cost separation technique in case of chromatography. Quality control laboratories have to develop and validate suitable analytical procedures in order to assay such multi component preparations. New spectrophotometric methods for the simultaneous determination of simvastatin (SIM) and nicotinic acid (NIA) in binary combinations were developed. These methods are based on chemometric treatment of data, the applied chemometric techniques are multivariate methods including classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS). In these techniques, the concentration data matrix were prepared by using the synthetic mixtures containing SIM and NIA dissolved in ethanol. The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbance at 12 wavelengths in the range 216 - 240 nm at 2 nm intervals in the zero-order. The spectrophotometric procedures do not require any separation step. The accuracy, precision and the linearity ranges of the methods have been determined and validated by analyzing synthetic mixtures containing the studied drugs. Chemometric spectrophotometric methods have been developed in the present study for the simultaneous determination of simvastatin and nicotinic acid in their synthetic binary mixtures and in their mixtures with possible excipients present in tablet dosage form. The validation was performed successfully. The developed methods have been shown to be accurate, linear, precise, and so simple. The developed methods can be used routinely for the determination dosage form. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Rapid and direct spectrophotometric method for kinetics studies and routine assay of peroxidase based on aniline diazo substrates.

PubMed

Mirazizi, Fatemeh; Bahrami, Azita; Haghbeen, Kamahldin; Shahbani Zahiri, Hossein; Bakavoli, Mehdi; Legge, Raymond L

2016-12-01

Peroxidases are ubiquitous enzymes that play an important role in living organisms. Current spectrophotometrically based peroxidase assay methods are based on the production of chromophoric substances at the end of the enzymatic reaction. The ambiguity regarding the formation and identity of the final chromophoric product and its possible reactions with other molecules have raised concerns about the accuracy of these methods. This can be of serious concern in inhibition studies. A novel spectrophotometric assay for peroxidase, based on direct measurement of a soluble aniline diazo substrate, is introduced. In addition to the routine assays, this method can be used in comprehensive kinetics studies. 4-[(4-Sulfophenyl)azo]aniline (λmax = 390 nm, ɛ = 32 880 M(-1) cm(-1) at pH 4.5 to 9) was introduced for routine assay of peroxidase. This compound is commercially available and is indexed as a food dye. Using this method, a detection limit of 0.05 nmol mL(-1) was achieved for peroxidase.

Development of normalized spectra manipulating spectrophotometric methods for simultaneous determination of Dimenhydrinate and Cinnarizine binary mixture.

PubMed

Lamie, Nesrine T; Yehia, Ali M

2015-01-01

Simultaneous determination of Dimenhydrinate (DIM) and Cinnarizine (CIN) binary mixture with simple procedures were applied. Three ratio manipulating spectrophotometric methods were proposed. Normalized spectrum was utilized as a divisor for simultaneous determination of both drugs with minimum manipulation steps. The proposed methods were simultaneous constant center (SCC), simultaneous derivative ratio spectrophotometry (S(1)DD) and ratio H-point standard addition method (RHPSAM). Peak amplitudes at isoabsorptive point in ratio spectra were measured for determination of total concentrations of DIM and CIN. For subsequent determination of DIM concentration, difference between peak amplitudes at 250 nm and 267 nm were used in SCC. While the peak amplitude at 275 nm of the first derivative ratio spectra were used in S(1)DD; then subtraction of DIM concentration from the total one provided the CIN concentration. The last RHPSAM was a dual wavelength method in which two calibrations were plotted at 220 nm and 230 nm. The coordinates of intersection point between the two calibration lines were corresponding to DIM and CIN concentrations. The proposed methods were successfully applied for combined dosage form analysis, Moreover statistical comparison between the proposed and reported spectrophotometric methods was applied. Copyright © 2015 Elsevier B.V. All rights reserved.

Bivariate versus multivariate smart spectrophotometric calibration methods for the simultaneous determination of a quaternary mixture of mosapride, pantoprazole and their degradation products.

PubMed

Hegazy, M A; Yehia, A M; Moustafa, A A

2013-05-01

The ability of bivariate and multivariate spectrophotometric methods was demonstrated in the resolution of a quaternary mixture of mosapride, pantoprazole and their degradation products. The bivariate calibrations include bivariate spectrophotometric method (BSM) and H-point standard addition method (HPSAM), which were able to determine the two drugs, simultaneously, but not in the presence of their degradation products, the results showed that simultaneous determinations could be performed in the concentration ranges of 5.0-50.0 microg/ml for mosapride and 10.0-40.0 microg/ml for pantoprazole by bivariate spectrophotometric method and in the concentration ranges of 5.0-45.0 microg/ml for both drugs by H-point standard addition method. Moreover, the applied multivariate calibration methods were able for the determination of mosapride, pantoprazole and their degradation products using concentration residuals augmented classical least squares (CRACLS) and partial least squares (PLS). The proposed multivariate methods were applied to 17 synthetic samples in the concentration ranges of 3.0-12.0 microg/ml mosapride, 8.0-32.0 microg/ml pantoprazole, 1.5-6.0 microg/ml mosapride degradation products and 2.0-8.0 microg/ml pantoprazole degradation products. The proposed bivariate and multivariate calibration methods were successfully applied to the determination of mosapride and pantoprazole in their pharmaceutical preparations.

Method for removal of phosgene from boron trichloride. [DOE patent application; mercury arc lamp

DOEpatents

Freund, S.M.

1981-09-03

Selective ultraviolet photolysis using an unfiltered mercury arc lamp has been used to substantially reduce the phosgene impurity in a mixture of boron trichloride and phosgene. Infrared spectrophotometric analysis of the sample before and after irradiation shows that it is possible to highly purify commercially available boron trichloride with this method.

Net analyte signal standard addition method (NASSAM) as a novel spectrofluorimetric and spectrophotometric technique for simultaneous determination, application to assay of melatonin and pyridoxine

NASA Astrophysics Data System (ADS)

Asadpour-Zeynali, Karim; Bastami, Mohammad

2010-02-01

In this work a new modification of the standard addition method called "net analyte signal standard addition method (NASSAM)" is presented for the simultaneous spectrofluorimetric and spectrophotometric analysis. The proposed method combines the advantages of standard addition method with those of net analyte signal concept. The method can be applied for the determination of analyte in the presence of known interferents. The accuracy of the predictions against H-point standard addition method is not dependent on the shape of the analyte and interferent spectra. The method was successfully applied to simultaneous spectrofluorimetric and spectrophotometric determination of pyridoxine (PY) and melatonin (MT) in synthetic mixtures and in a pharmaceutical formulation.

A Peroxidase-linked Spectrophotometric Assay for the Detection of Monoamine Oxidase Inhibitors.

PubMed

Zhi, Kangkang; Yang, Zhongduo; Sheng, Jie; Shu, Zongmei; Shi, Yin

2016-01-01

To develop a new more accurate spectrophotometric method for detecting monoamine oxidase inhibitors from plant extracts, a series of amine substrates were selected and their ability to be oxidized by monoamine oxidase was evaluated by the HPLC method and a new substrate was used to develop a peroxidase-linked spectrophotometric assay. 4-(Trifluoromethyl) benzylamine (11) was proved to be an excellent substrate for peroxidase-linked spectrophotometric assay. Therefore, a new peroxidase-linked spectrophotometric assay was set up. The principle of the method is that the MAO converts 11 into aldehyde, ammonia and hydrogen peroxide. In the presence of peroxidase, the hydrogen peroxide will oxidize 4-aminoantipyrine into oxidised 4-aminoantipyrine which can condense with vanillic acid to give a red quinoneimine dye. The production of the quinoneimine dye was detected at 490 nm by a microplate reader. The ⊿OD value between the blank group and blank negative control group in this new method is twice as much as that in Holt's method, which enables the procedure to be more accurate and avoids the produce of false positive results. The new method will be helpful for researchers to screening monoamine oxidase inhibitors from deep-color plant extracts.

Validation of a spectrophotometric method for quantification of carboxyhemoglobin.

PubMed

Luchini, Paulo D; Leyton, Jaime F; Strombech, Maria de Lourdes C; Ponce, Julio C; Jesus, Maria das Graças S; Leyton, Vilma

2009-10-01

The measurement of carboxyhemoglobin (COHb) levels in blood is a valuable procedure to confirm exposure to carbon monoxide (CO) either for forensic or occupational matters. A previously described method using spectrophotometric readings at 420 and 432 nm after reduction of oxyhemoglobin (O(2)Hb) and methemoglobin with sodium hydrosulfite solution leads to an exponential curve. This curve, used with pre-established factors, serves well for lower concentrations (1-7%) or for high concentrations (> 20%) but very rarely for both. The authors have observed that small variations on the previously described factors F1, F2, and F3, obtained from readings for 100% COHb and 100% O(2)Hb, turn into significant changes in COHb% results and propose that these factors should be determined every time COHb is measured by reading CO and O(2) saturated samples. This practice leads to an increase in accuracy and precision.

Novel spectrophotometric determination of flumethasone pivalate and clioquinol in their binary mixture and pharmaceutical formulation.

PubMed

Abdel-Aleem, Eglal A; Hegazy, Maha A; Sayed, Nour W; Abdelkawy, M; Abdelfatah, Rehab M

2015-02-05

This work is concerned with development and validation of three simple, specific, accurate and precise spectrophotometric methods for determination of flumethasone pivalate (FP) and clioquinol (CL) in their binary mixture and ear drops. Method A is a ratio subtraction spectrophotometric one (RSM). Method B is a ratio difference spectrophotometric one (RDSM), while method C is a mean center spectrophotometric one (MCR). The calibration curves are linear over the concentration range of 3-45 μg/mL for FP, and 2-25 μg/mL for CL. The specificity of the developed methods was assessed by analyzing different laboratory prepared mixtures of the FP and CL. The three methods were validated as per ICH guidelines; accuracy, precision and repeatability are found to be within the acceptable limits. Copyright © 2014 Elsevier B.V. All rights reserved.

Development and Validation of Eco-Friendly Liquid Chromatographic and Spectrophotometric Methods for Simultaneous Determination of Coformulated Drugs: Phenylephrine Hydrochloride and Prednisolone Acetate.

PubMed

Mostafa, Nadia M; Elsayed, Ghada M; Hassan, Nagiba Y; El Mously, Dina A

2017-11-01

Five simple, sensitive, and eco-friendly LC and UV spectrophotometric methods have been developed for the simultaneous determination of phenylephrine hydrochloride (PHE) and prednisolone acetate (PRD) in their combined dosage form. The first method was reversed-phase (RP) LC using methanol-water-heptane-1-sulfonic acid sodium salt (75 + 25 + 0.1, v/v/w) as a mobile phase. Separation was achieved using an XSelect HSS reversed-phase C18 analytical column (250 × 4.6 mm, 5µm). The flow rate was 1.0 mL/min and UV detection was done at 230 nm. Quantification was achieved over the concentration ranges of 5-50 µg/mL for PHE and 2-90 µg/mL for PRD. Four spectrophotometric methods were proposed, namely dual wavelength, first derivative of ratio spectra, ratio difference, and mean-centering of ratio spectra. Linearity was observed in the concentration ranges of 10-120 and 5-35 µg/mL for PHE and PRD, respectively, for the spectrophotometric methods. Green solvents were used in the proposed methods because they play a vital role in the analytical methods' influence on the environment. The suggested methods were validated regarding linearity, accuracy, and precision according to the International Conference on Harmonization guidelines, with satisfactory results. These methods could be used as harmless substitutes for routine analysis of the mentioned drugs, with no interference from excipients.

A new innovative spectrophotometric method for the simultaneous determination of sofosbuvir and ledipasvir

NASA Astrophysics Data System (ADS)

Mansour, Fotouh R.

2018-01-01

A new innovative spectrophotometric method is developed to determine the concentration ratios in binary mixtures by determining the zero crossing point in the first derivative of the gross curve. This relationship can be applied if the part of the UV spectrum of substance Y, that intersects with the overlaid spectra of substance X is straight. By plotting the intersection wavelength against the concentration ratio (Cx/Cy), a straight line was obtained with a co-efficient of determination equals 0.9999. As an application, simultaneous determination of sofosbuvir and ledipasvir in their binary mixtures was performed using two methods; a direct UV spectrophotometric method for determination of ledipasvir at 333 nm, and the new "wavelength-intersection ratio" method for determination of sofosbuvir. In the wavelength-intersection ratio method, different mixtures of sofosbuvir and ledipasvir containing different concentration ratios were prepared; the zero crossing point of the first derivative curve in the range 285 to 295 nm were determined for each mixture. An absorbance shift in the intersection was obtained with the change in the concentration ratio (sofosbuvir/ledipasvir). When the concentration ratio was plotted against the intersection wavelength, a straight line was obtained with a coefficient of determination of 0.9992. The direct method was linear in the range 3 to 18 μg/mL while the wavelength-intersection ratio method was linear in the range 11-110 μg/mL. The limits of detection were determined and found to be 0.5 and 3 μg/mL for ledipasvir and sofosbuvir, respectively. The accuracy and repeatability of the two methods were tested. The mean %recovery was found to be 100.19% and 100.75% for ledipasvir and sofosbuvir, respectively. The relative standard deviation was 0.57 for ledipasvir and 1.79 for sofosbuvir. The intermediate precision was also checked, the coefficients of variation for sofosbuvir and ledipasvir measurements between days did not exceed 1.88%.

Quantitative Analysis of Clopidogrel Bisulphate and Aspirin by First Derivative Spectrophotometric Method in Tablets

PubMed Central

Game, Madhuri D.; Gabhane, K. B.; Sakarkar, D. M.

2010-01-01

A simple, accurate and precise spectrophotometric method has been developed for simultaneous estimation of clopidogrel bisulphate and aspirin by employing first order derivative zero crossing method. The first order derivative absorption at 232.5 nm (zero cross point of aspirin) was used for clopidogrel bisulphate and 211.3 nm (zero cross point of clopidogrel bisulphate) for aspirin.Both the drugs obeyed linearity in the concentration range of 5.0 μg/ml to 25.0 μg/ml (correlation coefficient r2<1). No interference was found between both determined constituents and those of matrix. The method was validated statistically and recovery studies were carried out to confirm the accuracy of the method. PMID:21969765

Validated spectrophotometric method for the determination, spectroscopic characterization and thermal structural analysis of duloxetine with 1,2-naphthoquinone-4-sulphonate

NASA Astrophysics Data System (ADS)

Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

2012-03-01

A novel, selective, sensitive and simple spectrophotometric method was developed and validated for the determination of the antidepressant duloxetine hydrochloride in pharmaceutical preparation. The method was based on the reaction of duloxetine hydrochloride with 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline media to yield orange colored product. The formation of this complex was also confirmed by UV-visible, FTIR, 1H NMR, Mass spectra techniques and thermal analysis. This method was validated for various parameters according to ICH guidelines. Beer's law is obeyed in a range of 5.0-60 μg/mL at the maximum absorption wavelength of 480 nm. The detection limit is 0.99 μg/mL and the recovery rate is in a range of 98.10-99.57%. The proposed methods was validated and applied to the determination of duloxetine hydrochloride in pharmaceutical preparation. The results were statistically analyzed and compared to those of a reference UV spectrophotometric method.

Roles of reactive oxygen species in UVA-induced oxidation of 5,6-dihydroxyindole-2-carboxylic acid-melanin as studied by differential spectrophotometric method.

PubMed

Ito, Shosuke; Kikuta, Marina; Koike, Shota; Szewczyk, Grzegorz; Sarna, Michal; Zadlo, Andrzej; Sarna, Tadeusz; Wakamatsu, Kazumasa

2016-05-01

Eumelanin photoprotects pigmented tissues from ultraviolet (UV) damage. However, UVA-induced tanning seems to result from the photooxidation of preexisting melanin and does not contribute to photoprotection. We investigated the mechanism of UVA-induced degradation of 5,6-dihydroxyindole-2-carboxylic acid (DHICA)-melanin taking advantage of its solubility in a neutral buffer and using a differential spectrophotometric method to detect subtle changes in its structure. Our methodology is suitable for examining the effects of various agents that interact with reactive oxygen species (ROS) to determine how ROS is involved in the UVA-induced oxidative modifications. The results show that UVA radiation induces the oxidation of DHICA to indole-5,6-quinone-2-carboxylic acid in eumelanin, which is then cleaved to form a photodegraded, pyrrolic moiety and finally to form free pyrrole-2,3,5-tricarboxylic acid. The possible involvement of superoxide radical and singlet oxygen in the oxidation was suggested. The generation and quenching of singlet oxygen by DHICA-melanin was confirmed by direct measurements of singlet oxygen phosphorescence. © 2016 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

A Peroxidase-linked Spectrophotometric Assay for the Detection of Monoamine Oxidase Inhibitors

PubMed Central

Zhi, Kangkang; Yang, Zhongduo; Sheng, Jie; Shu, Zongmei; Shi, Yin

2016-01-01

To develop a new more accurate spectrophotometric method for detecting monoamine oxidase inhibitors from plant extracts, a series of amine substrates were selected and their ability to be oxidized by monoamine oxidase was evaluated by the HPLC method and a new substrate was used to develop a peroxidase-linked spectrophotometric assay. 4-(Trifluoromethyl) benzylamine (11) was proved to be an excellent substrate for peroxidase-linked spectrophotometric assay. Therefore, a new peroxidase-linked spectrophotometric assay was set up. The principle of the method is that the MAO converts 11 into aldehyde, ammonia and hydrogen peroxide. In the presence of peroxidase, the hydrogen peroxide will oxidize 4-aminoantipyrine into oxidised 4-aminoantipyrine which can condense with vanillic acid to give a red quinoneimine dye. The production of the quinoneimine dye was detected at 490 nm by a microplate reader. The ⊿OD value between the blank group and blank negative control group in this new method is twice as much as that in Holt’s method, which enables the procedure to be more accurate and avoids the produce of false positive results. The new method will be helpful for researchers to screening monoamine oxidase inhibitors from deep-color plant extracts. PMID:27610153

Application of the ratio difference spectrophotometry to the determination of ibuprofen and famotidine in their combined dosage form: comparison with previously published spectrophotometric methods.

PubMed

Zaazaa, Hala E; Elzanfaly, Eman S; Soudi, Aya T; Salem, Maissa Y

2015-05-15

Ratio difference spectrophotometric method was developed for the determination of ibuprofen and famotidine in their mixture form. Ibuprofen and famotidine were determined in the presence of each other by the ratio difference spectrophotometric (RD) method where linearity was obtained from 50 to 600μg/mL and 2.5 to 25μg/mL for ibuprofen and famotidine, respectively. The suggested method was validated according to ICH guidelines and successfully applied for the analysis of ibuprofen and famotidine in their pharmaceutical dosage forms without interference from any additives or excipients. Copyright © 2015 Elsevier B.V. All rights reserved.

Method for generating extreme ultraviolet with mather-type plasma accelerators for use in Extreme Ultraviolet Lithography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hassanein, Ahmed; Konkashbaev, Isak

A device and method for generating extremely short-wave ultraviolet electromagnetic wave uses two intersecting plasma beams generated by two plasma accelerators. The intersection of the two plasma beams emits electromagnetic radiation and in particular radiation in the extreme ultraviolet wavelength. In the preferred orientation two axially aligned counter streaming plasmas collide to produce an intense source of electromagnetic radiation at the 13.5 nm wavelength. The Mather type plasma accelerators can utilize tin, or lithium covered electrodes. Tin, lithium or xenon can be used as the photon emitting gas source.

Determination of total antioxidant capacity by a new spectrophotometric method based on Ce(IV) reducing capacity measurement.

PubMed

Ozyurt, Dilek; Demirata, Birsen; Apak, Resat

2007-02-28

Dietary antioxidants widely found in fruits and vegetables may serve the task of reducing oxidative damage in humans induced by free radicals and reactive oxygen species under 'oxidative stress' conditions. The aim of this work is to develop a simple, low-cost, sensitive, and diversely applicable indirect spectrophotometric method for the determination of total antioxidant capacity of several plants. The method is based on the oxidation of antioxidants with cerium(IV) sulfate in dilute sulfuric acid at room temperature. The Ce(IV) reducing capacity of the sample is measured under carefully adjusted conditions of oxidant concentration and pH such that only antioxidants and not other organic compounds would be oxidized. The spectrophotometric determination of the remaining Ce(IV) was performed after completion of reaction with antioxidants. Quercetin and gallic acid were used as standards for flavonoids and phenolic acids, respectively, and results of antioxidant measurements were reported as trolox equivalents. The developed procedure was successfully applied to the assay of total antioxidant capacity due to simple compounds such as trolox, quercetin, gallic acid, ascorbic acid, catechin, naringin, naringenin, caffeic acid, chlorogenic acid, ferulic acid, and p-coumaric acid, and due to phenolic acids and flavonoids in the arieal parts of nettle (Urtica Dioica L.). Blank correction of significantly absorbing plant extracts at 320nm could be made with the aid of spectrophotometric titration. Plant selection was made in respect to high antioxidant content, and extraction was made with water. The proposed method was reproducible, and the trolox equivalent antioxidant capacities (TEAC coefficients) of the tested antioxidant compounds were correlated to those found by reference methods such as ABTS and CUPRAC. Since the TEAC coefficients found with the proposed method of naringin-naringenin and rutin-catechin pairs were close to each other, this Ce(IV)-based assay

Determination of cyanide by a highly sensitive indirect spectrophotometric method.

PubMed

Blanco, M; Maspoch, S

1984-01-01

Complexation of Pd(2+) with cyanide inhibits the extraction of the palladium complex of 5-phenylazo-8-aminoquinoline. This effect is used for the indirect spectrophotometric determination of cyanide at the mug level. Cyanide in industrial waste water and in sea-water is determined after distillation as HCN from the sample and collection in sodium hydroxide solution.

Development and validation of spectrophotometric methods for estimating amisulpride in pharmaceutical preparations.

PubMed

Sharma, Sangita; Neog, Madhurjya; Prajapati, Vipul; Patel, Hiren; Dabhi, Dipti

2010-01-01

Five simple, sensitive, accurate and rapid visible spectrophotometric methods (A, B, C, D and E) have been developed for estimating Amisulpride in pharmaceutical preparations. These are based on the diazotization of Amisulpride with sodium nitrite and hydrochloric acid, followed by coupling with N-(1-naphthyl)ethylenediamine dihydrochloride (Method A), diphenylamine (Method B), beta-naphthol in an alkaline medium (Method C), resorcinol in an alkaline medium (Method D) and chromotropic acid in an alkaline medium (Method E) to form a colored chromogen. The absorption maxima, lambda(max), are at 523 nm for Method A, 382 and 490 nm for Method B, 527 nm for Method C, 521 nm for Method D and 486 nm for Method E. Beer's law was obeyed in the concentration range of 2.5-12.5 microg mL(-1) in Method A, 5-25 and 10-50 microg mL(-1) in Method B, 4-20 microg mL(-1) in Method C, 2.5-12.5 microg mL(-1) in Method D and 5-15 microg mL(-1) in Method E. The results obtained for the proposed methods are in good agreement with labeled amounts, when marketed pharmaceutical preparations were analyzed.

Development and Validation of Stability-Indicating Derivative Spectrophotometric Methods for Determination of Dronedarone Hydrochloride

NASA Astrophysics Data System (ADS)

Chadha, R.; Bali, A.

2016-05-01

Rapid, sensitive, cost effective and reproducible stability-indicating derivative spectrophotometric methods have been developed for the estimation of dronedarone HCl employing peak-zero (P-0) and peak-peak (P-P) techniques, and their stability-indicating potential assessed in forced degraded solutions of the drug. The methods were validated with respect to linearity, accuracy, precision and robustness. Excellent linearity was observed in concentrations 2-40 μg/ml ( r 2 = 0.9986). LOD and LOQ values for the proposed methods ranged from 0.42-0.46 μg/ml and 1.21-1.27 μg/ml, respectively, and excellent recovery of the drug was obtained in the tablet samples (99.70 ± 0.84%).

The measurement of acetanilide in plasma by spectrophotometric and selected ion monitoring methods.

PubMed

Baty, J D; Playfer, J; Evans, D A; Lamb, J

1977-08-01

Plasma samples from volunteers who had received an oral dose of acetanilide have been analysed by gas chromatography mass spectrometry and ultraviolet absorption techniques. The gas chromatography mass spectrometry method involved extraction of the plasma and analysis of the acetanilide using selected ion monitoring with a deuterated internal standard. In the ultraviolet method the plasma was hydrolysed with acid to convert the acetanilide to aniline, and this compound was diazotized and coupled with N-1-naphthylethylene-diamine. The absorbance of the resulting complex was read at 550 nm. Acetanilide levels in plasma determined by the selected ion monitoring method were significantly lower than those measured by spectrophotometry. Pharmacokinetic data calculated from the results obtained using these two assays are very different and illustrate the need for an accurate and specific method of analysis. The major metabolites of acetanilide are shown not to interfere with these assays and the results suggest the possible presence of a new metabolite of acetanilide.

A study of selective spectrophotometric methods for simultaneous determination of Itopride hydrochloride and Rabeprazole sodium binary mixture: Resolving sever overlapping spectra

NASA Astrophysics Data System (ADS)

Mohamed, Heba M.

2015-02-01

Itopride hydrochloride (IT) and Rabeprazole sodium (RB) are co-formulated together for the treatment of gastro-esophageal reflux disease. Three simple, specific and accurate spectrophotometric methods were applied and validated for simultaneous determination of Itopride hydrochloride (IT) and Rabeprazole sodium (RB) namely; constant center (CC), ratio difference (RD) and mean centering of ratio spectra (MCR) spectrophotometric methods. Linear correlations were obtained in range of 10-110 μg/μL for Itopride hydrochloride and 4-44 μg/mL for Rabeprazole sodium. No preliminary separation steps were required prior the analysis of the two drugs using the proposed methods. Specificity was investigated by analyzing the synthetic mixtures containing the two cited drugs and their capsules dosage form. The obtained results were statistically compared with those obtained by the reported method, no significant difference was obtained with respect to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for IT and RB.

Comparison of Two Spectrophotometric Techniques for Nutrients Analyses in Water Samples

NASA Astrophysics Data System (ADS)

Bartošová, Alica; Michalíková, Anna; Sirotiak, Maroš; Soldán, Maroš

2013-01-01

The aim of this contribution is to compare two common techniques for determining the concentrations of nitrate, nitrite, ammonium and phosphates in surface water and groundwater. Excess of these nutrients in water can directly affect human health (e.g. methemoglobinaemia) or indirectly through the products of secondary pollution - eutrophication (e.g. cyanotoxins, emanation of hydrogen sulphide, mercaptanes, methane...). Negative impact of nutrients excess in surface water often causes the destruction of water ecosystems, and therefore, common substances of these elements must be monitored and managed. For these experiments two spectrophotometric techniques - ultraviolet spectrophotometry and nutrient photometry were used. These techniques are commonly used for quick and simple analyses of nutrients in waste water. There are calibration curves for each nutrient and for determination of their concentration.

Development and validation of sensitive kinetic spectrophotometric method for the determination of moxifloxacin antibiotic in pure and commercial tablets

NASA Astrophysics Data System (ADS)

Ashour, Safwan; Bayram, Roula

2015-04-01

New, accurate, sensitive and reliable kinetic spectrophotometric method for the assay of moxifloxacin hydrochloride (MOXF) in pure form and pharmaceutical formulations has been developed. The method involves the oxidative coupling reaction of MOXF with 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) in the presence of Ce(IV) in an acidic medium to form colored product with lambda max at 623 and 660 nm. The reaction is followed spectrophotometrically by measuring the increase in absorbance at 623 nm as a function of time. The initial rate and fixed time methods were adopted for constructing the calibration curves. The linearity range was found to be 1.89-40.0 μg mL-1 for initial rate and fixed time methods. The limit of detection for initial rate and fixed time methods is 0.644 and 0.043 μg mL-1, respectively. Molar absorptivity for the method was found to be 0.89 × 104 L mol-1 cm-1. Statistical treatment of the experimental results indicates that the methods are precise and accurate. The proposed method has been applied successfully for the estimation of moxifloxacin hydrochloride in tablet dosage form with no interference from the excipients. The results are compared with the official method.

Development and validation of liquid chromatographic and UV derivative spectrophotometric methods for the determination of famciclovir in pharmaceutical dosage forms.

PubMed

Srinubabu, Gedela; Sudharani, Batchu; Sridhar, Lade; Rao, Jvln Seshagiri

2006-06-01

A high-performance liquid chromatographic method and a UV derivative spectrophotometric method for the determination of famciclovir, a highly active antiviral agent, in tablets were developed in the present work. The various parameters, such as linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. HPLC was carried out by using the reversed-phase technique on an RP-18 column with a mobile phase composed of 50 mM monobasic phosphate buffer and methanol (50 : 50; v/v), adjusted to pH 3.05 with orthophosphoric acid. The mobile phase was pumped at a flow rate of 1 ml/min and detection was made at 242 nm with UV dual absorbance detector. The first derivative UV spectrophotometric method was performed at 226.5 nm. Statistical analysis was done by Student's t-test and F-test, which showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and therefore can be used for its Intended purpose.

Spectrophotometric determination of 4-acetamidophenyl N'-(sulphanilamide) acetate in biological fluids.

PubMed

Shah, Bhavna; Patil, Pravin; Shah, Hirva

2014-01-01

A simple, accurate and low cost spectrophotometric method is proposed for the determination of the synthesized paracetamol derivative; 4-acetamidophenyl N'-(sulphanilamide) acetate (APSA) in biological fluids. The spectrophotometric method is based on a condensation reaction between the alcoholic solution of APSA and acidic solution of p-dimethylaminobenzaldeyde (DPMK) to generate a yellow colored product. The linear range for the determination of APSA was 1-10 µg mL(-1) with molar absorptivity of 3.6877 × 10(4) L mol(-1) cm(-1) and Sandell's sensitivity of 0.001 µg cm-2/0.001 absorbance unit. During the inter-day and intra-day analysis, the relative standard deviation for replicated determination of APSA was found to be less than 2.0% and accuracy was 99.20-101.60% and 99.10-101.30% in blood and urine samples, respectively. There was no interference with commonly used blood and urine sample. The developed spectrophotometric method was successfully applied to assess APSA in biological fluids.

Investigation of different spectrophotometric and chemometric methods for determination of entacapone, levodopa and carbidopa in ternary mixture

NASA Astrophysics Data System (ADS)

Abdel-Ghany, Maha F.; Hussein, Lobna A.; Ayad, Miriam F.; Youssef, Menatallah M.

2017-01-01

New, simple, accurate and sensitive UV spectrophotometric and chemometric methods have been developed and validated for determination of Entacapone (ENT), Levodopa (LD) and Carbidopa (CD) in ternary mixture. Method A is a derivative ratio spectra zero-crossing spectrophotometric method which allows the determination of ENT in the presence of both LD and CD by measuring the peak amplitude at 249.9 nm in the range of 1-20 μg mL- 1. Method B is a double divisor-first derivative of ratio spectra method, used for determination of ENT, LD and CD at 245, 239 and 293 nm, respectively. Method C is a mean centering of ratio spectra which allows their determination at 241, 241.6 and 257.1 nm, respectively. Methods B and C could successfully determine the studied drugs in concentration ranges of 1-20 μg mL- 1 for ENT and 10-90 μg mL- 1 for both LD and CD. Methods D and E are principal component regression and partial least-squares, respectively, used for the simultaneous determination of the studied drugs by using seventeen mixtures as calibration set and eight mixtures as validation set. The developed methods have the advantage of simultaneous determination of the cited components without any pre-treatment. All the results were statistically compared with the reported methods, where no significant difference was observed. The developed methods were satisfactorily applied to the analysis of the investigated drugs in their pure form and in pharmaceutical dosage forms.

Spectrophotometric method development and validation for determination of chlorpheniramine maleate in bulk and controlled release tablets.

PubMed

Ashfaq, Maria; Sial, Ali Akber; Bushra, Rabia; Rehman, Atta-Ur; Baig, Mirza Tasawur; Huma, Ambreen; Ahmed, Maryam

2018-01-01

Spectrophotometric technique is considered to be the simplest and operator friendly among other available analytical methods for pharmaceutical analysis. The objective of the study was to develop a precise, accurate and rapid UV-spectrophotometric method for the estimation of chlorpheniramine maleate (CPM) in pure and solid pharmaceutical formulation. Drug absorption was measured in various solvent systems including 0.1N HCl (pH 1.2), acetate buffer (pH 4.5), phosphate buffer (pH 6.8) and distil water (pH 7.0). Method validation was performed as per official guidelines of ICH, 2005. High drug absorption was observed in 0.1N HCl medium with λ max of 261nm. The drug showed the good linearity from 20 to 60μg/mL solution concentration with the correlation coefficient linear regression equation Y= 0.1853 X + 0.1098 presenting R 2 value of 0.9998. The method accuracy was evaluated by the percent drug recovery, presents more than 99% drug recovery at three different levels assessed. The % RSD value <1 was computed for inter and intraday analysis indicating the high accuracy and precision of the developed technique. The developed method is robust because it shows no any significant variation in with minute changes. The LOD and LOQ values were assessed to be 2.2μg/mL and 6.6μg/mL respectively. The investigated method proved its sensitivity, precision and accuracy hence could be successfully used to estimate the CPM content in bulk and pharmaceutical matrix tablets.

Analysis of ultraviolet spectrophotometric data from Copernicus. Final report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Snow, T.P. Jr

1979-04-17

Ultraviolet spectral data from the OAO 3 satellite are being used to study interstellar absorption lines and stellar and circumstellar lines in hot stars. The interstellar data are beneficial in analyzing the depletions of heavy elements from the gas phase and in elucidating how these depletions depend on physical conditions. Abundances in separate velocity components were determined from line profiles. Observations were carried out for interstellar abundances, both atomic and molecular, towards a number of stars. The better quality data are being analyzed for profile information and the lesser data are being used in curve-of-growth analyses. Molecular observations were carriedmore » out as well; N/sup 2/ was sought, interstellar C/sup 2/ was detected and its rotational excitation utilized to establish limits in interstellar cloud temperatures. An extensive search for H/sup 2/O resulted in a tentative identification which will produce new information on chemical reaction rates. Interstellar depletions and grain properties in the rho Ophiuchi cloud, stellar wind variability, and circumstellar lines are also under study.« less

Validated stability-indicating spectrophotometric methods for the determination of cefixime trihydrate in the presence of its acid and alkali degradation products.

PubMed

Mostafa, Nadia M; Abdel-Fattah, Laila; Weshahy, Soheir A; Hassan, Nagiba Y; Boltia, Shereen A

2015-01-01

Five simple, accurate, precise, and economical spectrophotometric methods have been developed for the determination of cefixime trihydrate (CFX) in the presence of its acid and alkali degradation products without prior separation. In the first method, second derivative (2D) and first derivative (1D) spectrophotometry was applied to the absorption spectra of CFX and its acid (2D) or alkali (1D) degradation products by measuring the amplitude at 289 and 308 nm, respectively. The second method was a first derivative (1DD) ratio spectrophotometric method where the peak amplitudes were measured at 311 nm in presence of the acid degradation product, and 273 and 306 nm in presence of its alkali degradation product. The third method was ratio subtraction spectrophotometry where the drug is determined at 286 nm in laboratory-prepared mixtures of CFX and its acid or alkali degradation product. The fourth method was based on dual wavelength analysis; two wavelengths were selected at which the absorbances of one component were the same, so wavelengths 209 and 252 nm were used to determine CFX in presence of its acid degradation product and 310 and 321 nm in presence of its alkali degradation product. The fifth method was bivariate spectrophotometric calibration based on four linear regression equations obtained at the wavelengths 231 and 290 nm, and 231 and 285 nm for the binary mixture of CFX with either its acid or alkali degradation product, respectively. The developed methods were successfully applied to the analysis of CFX in laboratory-prepared mixtures and pharmaceutical formulations with good recoveries, and their validation was carried out following the International Conference on Harmonization guidelines. The results obtained were statistically compared with each other and showed no significant difference with respect to accuracy and precision.

Innovative spectrophotometric methods for simultaneous estimation of the novel two-drug combination: Sacubitril/Valsartan through two manipulation approaches and a comparative statistical study

NASA Astrophysics Data System (ADS)

Eissa, Maya S.; Abou Al Alamein, Amal M.

2018-03-01

Different innovative spectrophotometric methods were introduced for the first time for simultaneous quantification of sacubitril/valsartan in their binary mixture and in their combined dosage form without prior separation through two manipulation approaches. These approaches were developed and based either on two wavelength selection in zero-order absorption spectra namely; dual wavelength method (DWL) at 226 nm and 275 nm for valsartan, induced dual wavelength method (IDW) at 226 nm and 254 nm for sacubitril and advanced absorbance subtraction (AAS) based on their iso-absorptive point at 246 nm (λiso) and 261 nm (sacubitril shows equal absorbance values at the two selected wavelengths) or on ratio spectra using their normalized spectra namely; ratio difference spectrophotometric method (RD) at 225 nm and 264 nm for both of them in their ratio spectra, first derivative of ratio spectra (DR1) at 232 nm for valsartan and 239 nm for sacubitril and mean centering of ratio spectra (MCR) at 260 nm for both of them. Both sacubitril and valsartan showed linearity upon application of these methods in the range of 2.5-25.0 μg/mL. The developed spectrophotmetric methods were successfully applied to the analysis of their combined tablet dosage form ENTRESTO™. The adopted spectrophotometric methods were also validated according to ICH guidelines. The results obtained from the proposed methods were statistically compared to a reported HPLC method using Student t-test, F-test and a comparative study was also developed with one-way ANOVA, showing no statistical difference in accordance to precision and accuracy.

A New Kinetic Spectrophotometric Method for the Quantitation of Amorolfine.

PubMed

Soto, César; Poza, Cristian; Contreras, David; Yáñez, Jorge; Nacaratte, Fallon; Toral, M Inés

2017-01-01

Amorolfine (AOF) is a compound with fungicide activity based on the dual inhibition of growth of the fungal cell membrane, the biosynthesis and accumulation of sterols, and the reduction of ergosterol. In this work a sensitive kinetic and spectrophotometric method for the AOF quantitation based on the AOF oxidation by means of KMnO 4 at 30 min (fixed time), pH alkaline, and ionic strength controlled was developed. Measurements of changes in absorbance at 610 nm were used as criterion of the oxidation progress. In order to maximize the sensitivity, different experimental reaction parameters were carefully studied via factorial screening and optimized by multivariate method. The linearity, intraday, and interday assay precision and accuracy were determined. The absorbance-concentration plot corresponding to tap water spiked samples was rectilinear, over the range of 7.56 × 10 -6 -3.22 × 10 -5  mol L -1 , with detection and quantitation limits of 2.49 × 10 -6  mol L -1 and 7.56 × 10 -6  mol L -1 , respectively. The proposed method was successfully validated for the application of the determination of the drug in the spiked tap water samples and the percentage recoveries were 94.0-105.0%. The method is simple and does not require expensive instruments or complicated extraction steps of the reaction product.

[Spectrophotometric and HPLC evaluation of ceftazidime stability].

PubMed

Palade, B; Cioroiu, B; Lazăr, Doina; Corciovă, Andreia; Lazăr, M I

2010-01-01

In this paper we followed up the stability of ceftazidime, raw material used in drug industry. Matherials and methods: We used three spectrophotometric methods based on ceftazidime property to form complexes with p-chloranilic acid (ac. p-CA), 3-methylbenzothiazolin-2-on hydrazone (MBTH) and N-(1-naphtil) etilendiamine (NEDA) and a chromatographic method (HPLC). Our results revealed that the substances analyzed maintained minimum content allowable.

Spectrophotometric reading of EUCAST antifungal susceptibility testing of Aspergillus fumigatus.

PubMed

Meletiadis, J; Leth Mortensen, K; Verweij, P E; Mouton, J W; Arendrup, M C

2017-02-01

Given the increasing number of antifungal drugs and the emergence of resistant Aspergillus isolates, objective, automated and high-throughput antifungal susceptibility testing is important. The EUCAST E.Def 9.3 reference method for MIC determination of Aspergillus species relies on visual reading. Spectrophotometric reading was not adopted because of concern that non-uniform filamentous growth might lead to unreliable and non-reproducible results. We therefore evaluated spectrophotometric reading for the determination of MICs of antifungal azoles against Aspergillus fumigatus. Eighty-eight clinical isolates of A. fumigatus were tested against four medical azoles (posaconazole, voriconazole, itraconazole, isavuconazole) and one agricultural azole (tebuconazole) with EUCAST E.Def 9.3. The visually determined MICs (complete inhibition of growth) were compared with spectrophotometrically determined MICs and essential (±1 twofold dilution) and categorical (susceptible/intermediate/resistant or wild-type/non-wild-type) agreement was calculated. Spectrophotometric data were analysed with regression analysis using the E max model, and the effective concentration corresponding to 5% (EC 5 ) was estimated. Using the 5% cut-off, high essential (92%-97%) and categorical (93%-99%) agreement (<6% errors) was found between spectrophotometric and visual MICs. The EC 5 also correlated with the visually determined MICs with an essential agreement of 83%-96% and a categorical agreement of 90%-100% (<5% errors). Spectrophotometric determination of MICs of antifungal drugs may increase objectivity, and allow automation and high-throughput of EUCAST E.Def 9.3 antifungal susceptibility testing of Aspergillus species. Copyright © 2016 European Society of Clinical Microbiology and Infectious Diseases. Published by Elsevier Ltd. All rights reserved.

Reliable samples of quasars and hot stars from a spectrophotometric survey of the U.S. catalogs

NASA Technical Reports Server (NTRS)

Mitchell, Kenneth J.

1987-01-01

The U.S. survey for blue- and ultraviolet-excess starlike objects is reviewed, focusing on the features which have contributed to its accuracy. The spectrophotometric survey is described in terms of the observational setup and procedures. It is suggested that the survey has produced reliably classified samples of quasars and hot evolved stars and that the procedures used in the study provide a means of deriving distance and luminosity information about these objects. Several cumulative number counts and spectra of a DA white dwarf and a quasar with prominent C IV and C III emission are given as examples.

A study of selective spectrophotometric methods for simultaneous determination of Itopride hydrochloride and Rabeprazole sodium binary mixture: Resolving sever overlapping spectra.

PubMed

Mohamed, Heba M

2015-02-05

Itopride hydrochloride (IT) and Rabeprazole sodium (RB) are co-formulated together for the treatment of gastro-esophageal reflux disease. Three simple, specific and accurate spectrophotometric methods were applied and validated for simultaneous determination of Itopride hydrochloride (IT) and Rabeprazole sodium (RB) namely; constant center (CC), ratio difference (RD) and mean centering of ratio spectra (MCR) spectrophotometric methods. Linear correlations were obtained in range of 10-110μg/μL for Itopride hydrochloride and 4-44μg/mL for Rabeprazole sodium. No preliminary separation steps were required prior the analysis of the two drugs using the proposed methods. Specificity was investigated by analyzing the synthetic mixtures containing the two cited drugs and their capsules dosage form. The obtained results were statistically compared with those obtained by the reported method, no significant difference was obtained with respect to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for IT and RB. Copyright © 2014 Elsevier B.V. All rights reserved.

Analytical method development and validation of spectrofluorimetric and spectrophotometric determination of some antimicrobial drugs in their pharmaceuticals.

PubMed

Ibrahim, F; Wahba, M E K; Magdy, G

2018-01-05

In this study, three novel, sensitive, simple and validated spectrophotometric and spectrofluorimetric methods have been proposed for estimation of some important antimicrobial drugs. The first two methods have been proposed for estimation of two important third-generation cephalosporin antibiotics namely, cefixime and cefdinir. Both methods were based on condensation of the primary amino group of the studied drugs with acetyl acetone and formaldehyde in acidic medium. The resulting products were measured by spectrophotometric (Method I) and spectrofluorimetric (Method II) tools. Regarding method I, the absorbance was measured at 315nm and 403nm with linearity ranges of 5.0-140.0 and 10.0-100.0μg/mL for cefixime and cefdinir, respectively. Meanwhile in method II, the produced fluorophore was measured at λ em 488nm or 491nm after excitation at λ ex 410nm with linearity ranges of 0.20-10.0 and 0.20-36.0μg/mL for cefixime and cefdinir, respectively. On the other hand, method III was devoted to estimate nifuroxazide spectrofluorimetrically depending on formation of highly fluorescent product upon reduction of the studied drug with Zinc powder in acidic medium. Measurement of the fluorescent product was carried out at λ em 335nm following excitation at λ ex 255nm with linearity range of 0.05 to 1.6μg/mL. The developed methods were subjected to detailed validation procedure, moreover they were used for the estimation of the concerned drugs in their pharmaceuticals. It was found that there is a good agreement between the obtained results and those obtained by the reported methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical method development and validation of spectrofluorimetric and spectrophotometric determination of some antimicrobial drugs in their pharmaceuticals

NASA Astrophysics Data System (ADS)

Ibrahim, F.; Wahba, M. E. K.; Magdy, G.

2018-01-01

In this study, three novel, sensitive, simple and validated spectrophotometric and spectrofluorimetric methods have been proposed for estimation of some important antimicrobial drugs. The first two methods have been proposed for estimation of two important third-generation cephalosporin antibiotics namely, cefixime and cefdinir. Both methods were based on condensation of the primary amino group of the studied drugs with acetyl acetone and formaldehyde in acidic medium. The resulting products were measured by spectrophotometric (Method I) and spectrofluorimetric (Method II) tools. Regarding method I, the absorbance was measured at 315 nm and 403 nm with linearity ranges of 5.0-140.0 and 10.0-100.0 μg/mL for cefixime and cefdinir, respectively. Meanwhile in method II, the produced fluorophore was measured at λem 488 nm or 491 nm after excitation at λex 410 nm with linearity ranges of 0.20-10.0 and 0.20-36.0 μg/mL for cefixime and cefdinir, respectively. On the other hand, method III was devoted to estimate nifuroxazide spectrofluorimetrically depending on formation of highly fluorescent product upon reduction of the studied drug with Zinc powder in acidic medium. Measurement of the fluorescent product was carried out at λem 335 nm following excitation at λex 255 nm with linearity range of 0.05 to 1.6 μg/mL. The developed methods were subjected to detailed validation procedure, moreover they were used for the estimation of the concerned drugs in their pharmaceuticals. It was found that there is a good agreement between the obtained results and those obtained by the reported methods.

Spectrophotometric determination of ketoprofen and its application in pharmaceutical analysis.

PubMed

Kormosh, Zholt; Hunka, Iryna; Basel, Yaroslav

2009-01-01

A new simple rapid and sensitive spectrophotometric method has been developed for the determination of ketoprofen in pharmaceutical preparations. The method is based on the reaction of ketoprofen with an analytical reagent--Astra Phloxin FF--at pH 8.0-10.8 and followed by the extraction of formed ion associate in toluene with spectrophotometric detection (it has an absorption maximum at 563 nm, epsilon = 7.6 x 10(4) L x mol(-1) x cm(-1)). The calibration plot was linear from 0.8-16.0 microg x mL(-1) of ketoprofen, and the detection limit was 0.037 microg x mL(-1).

Determination of moclobemide in human plasma by high-performance liquid chromatography with spectrophotometric detection.

PubMed

Amini, Hossein; Shahmir, Badri; Ahmadiani, Abolhassan

2004-08-05

A simple and sensitive high-performance liquid chromatographic (HPLC) method with spectrophotometric detection was developed for the determination of moclobemide in human plasma. Plasma samples were extracted under basic conditions with dichloromethane followed by back-extraction into diluted phosphoric acid. Isocratic separation was employed on an ODS column (250 mm x 4.6 mm, 5 microm) at room temperature. The mobile phase consisted of 5 mM NaH2PO4-acetonitrile-triethylamine (1000:350:10 (v/v/v), pH 3.4). Analyses were run at a flow-rate of 1.0 ml/min and ultraviolet (UV) detection was carried out at 240 nm. The method was specific and sensitive with a quantification limit of 15.6 ng/ml and a detection limit of 5 ng/ml at a signal-to-noise ratio of 3:1. The mean absolute recovery was about 98.2%, while the intra- and inter-day coefficient of variation and percent error values of the assay method were all at acceptable levels. Linearity was assessed in the range of 15.6-2000 ng/ml in plasma with a correlation coefficient of greater than 0.999. This method has been used to analyze several hundred human plasma samples for bioavailibility studies.

Catalog of far-ultraviolet objective-prism spectrophotometry: Skylab experiment S-019, ultraviolet steller astronomy

NASA Technical Reports Server (NTRS)

Henize, K. G.; Wray, J. D.; Parsons, S. B.; Benedict, G. F.

1979-01-01

Ultraviolet stellar spectra in the wavelength region from 1300 to 5000 A (130 to 500) were photographed during the three manned Skylab missions using a 15 cm aperture objective-prism telescope. The prismatic dispersion varied from 58 A mm/1 at 1400 A to 1600 A mm/1 at 3000 A. Approximately 1000 spectra representing 500 stars were measured and reduced to observed fluxes. About 100 stars show absorption lines of Si IV, C IV, or C II. Numerous line features are also recorded in supergiant stars, shell stars, A and F stars, and Wolf-Rayet stars. Most of the stars in the catalog are of spectral class B, with a number of O and A type stars and a sampling of WC, WN, F and C type stars. Spectrophotometric results are tabulated for these 500 stars.

Application of spectrophotometric, densitometric, and HPLC techniques as stability indicating methods for determination of Zaleplon in pharmaceutical preparations

NASA Astrophysics Data System (ADS)

Metwally, Fadia H.; Abdelkawy, M.; Abdelwahab, Nada S.

2007-12-01

Spectrophotometric, spectrodensitometric and HPLC are stability indicating methods described for determination of Zaleplon in pure and dosage forms. As Zaleplon is easily degradable, the proposed techniques in this manuscript are adopted for its determination in presence of its alkaline degradation product, namely N-[4-(3-cyano-pyrazolo[1,5a]pyridin-7-yl)-phenyl]- N-ethyl-acetamide. These approaches are successfully applied to quantify Zaleplon using the information included in the absorption spectra of appropriate solutions. The second derivative (D 2) spectrophotometric method, allows determination of Zaleplon without interference of its degradate at 235.2 nm using 0.01N HCl as a solvent with obedience to Beer's law over a concentration range of 1-10 μg ml -1 with mean percentage recovery 100.24 ± 0.86%. The first derivative of the ratio spectra ( 1DD) based on the simultaneous use of ( 1DD) and measurement at 241.8 nm using the same solvent and over the same concentration range as (D 2) spectrophotometric method, with mean percentage recovery 99.9 ± 1.07%. The spectrodensitometric analysis allows the separation and quantitation of Zaleplon from its degradate on silica gel plates using chloroform:acetone:ammonia solution (9:1:0.2 by volume) as a mobile phase. This method depends on quantitave densitometric evaluation of thin layer chromatogram of Zaleplon at 338 nm over a concentration range of 0.2-1 μg band -1, with mean percentage recovery 99.73 ± 1.35. Also a reversed-phase liquid chromatographic method using 5-C8 (22 cm × 4.6 mm i.d. 5 μm particle size) column was described and validated for quantitation of Zaleplon using acetonitrile:deionised water (35:65, v/v) as a mobile phase using Paracetamol as internal standard and a flow rate of 1.5 ml min -1 with UV detection of the effluent at 232 nm at ambient temperature over a concentration range of 2-20 μg ml -1 with mean percentage recovery 100.19 ± 1.15%. The insignificance difference of the proposed

A comparative study of the novel spectrophotometric methods versus conventional ones for the simultaneous determination of Esomeprazole magnesium trihydrate and Naproxen in their binary mixture.

PubMed

Lotfy, Hayam M; Amer, Sawsan M; Zaazaa, Hala E; Mostafa, Noha S

2015-01-01

Two novel simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed and validated for simultaneous determination of Esomeprazole magnesium trihydrate (ESO) and Naproxen (NAP) namely; absorbance subtraction and ratio difference. The results were compared to that of the conventional spectrophotometric methods namely; dual wavelength and isoabsorptive point coupled with first derivative of ratio spectra and derivative ratio. The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of ESO and NAP in their laboratory prepared mixtures and pharmaceutical preparation. No preliminary separation steps are required for the proposed spectrophotometeric procedures. The statistical comparison showed that there is no significant difference between the proposed methods and the reported method with respect to both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel Spectrophotometric Method for the Determination of Pindolol in Pharmaceutical Samples

NASA Astrophysics Data System (ADS)

Nagaraja, P.; Kumar, H. R. Arun; Bhaskara, B. L.; Kumar, S. Anil

2011-10-01

A new facile and sensitive spectrophotometric determination of Pindolol (PDL), a beta blocker drug has been developed and validated. The method was based on the reaction between pindolol and K3 [Fe(CN)6] in presence of FeCl3 to form Prussian blue. The absorbance values were recorded at 700 nm and a calibrated graph was constructed. A dynamic Beer's law range was observed in the range 0.125-2.5 μg mL-1 with a detection limit of 0.03 μg mL-1 and a quantitation limit of 0.08 μg mL-1. Various experimental parameters such as effect of solvents, stability, interference effects due to excipients etc were studied. The reproducibility of this methods were checked by six replicate determinations at 1.0 μg ml-1 PDL and the standard deviation was found to be between 0.20 and 0.42%. The results were statistically compared with those of the reference/literature method by applying Student's t-test and F-test. The sensitivity, simplicity, temperature independence and stability of the colored product are the advantages of the proposed method and it is also free from extraction steps and use of carcinogenic solvents.

Innovative spectrophotometric methods for simultaneous estimation of the novel two-drug combination: Sacubitril/Valsartan through two manipulation approaches and a comparative statistical study.

PubMed

Eissa, Maya S; Abou Al Alamein, Amal M

2018-03-15

Different innovative spectrophotometric methods were introduced for the first time for simultaneous quantification of sacubitril/valsartan in their binary mixture and in their combined dosage form without prior separation through two manipulation approaches. These approaches were developed and based either on two wavelength selection in zero-order absorption spectra namely; dual wavelength method (DWL) at 226nm and 275nm for valsartan, induced dual wavelength method (IDW) at 226nm and 254nm for sacubitril and advanced absorbance subtraction (AAS) based on their iso-absorptive point at 246nm (λ iso ) and 261nm (sacubitril shows equal absorbance values at the two selected wavelengths) or on ratio spectra using their normalized spectra namely; ratio difference spectrophotometric method (RD) at 225nm and 264nm for both of them in their ratio spectra, first derivative of ratio spectra (DR 1 ) at 232nm for valsartan and 239nm for sacubitril and mean centering of ratio spectra (MCR) at 260nm for both of them. Both sacubitril and valsartan showed linearity upon application of these methods in the range of 2.5-25.0μg/mL. The developed spectrophotmetric methods were successfully applied to the analysis of their combined tablet dosage form ENTRESTO™. The adopted spectrophotometric methods were also validated according to ICH guidelines. The results obtained from the proposed methods were statistically compared to a reported HPLC method using Student t-test, F-test and a comparative study was also developed with one-way ANOVA, showing no statistical difference in accordance to precision and accuracy. Copyright © 2017 Elsevier B.V. All rights reserved.

Spectrophotometric, spectrofluorimetric, and densitometric methods for the determination of indapamide.

PubMed

Youssef, Nadia F

2003-01-01

Three sensitive spectrophotometric, spectrofluorimetric, and densitometric methods are described for the determination of indapamide. The first and second methods are based on the oxidative coupling reaction of indapamide with 3-methyl-2-benzothiazolinone hydrazone HCl (MBTH) in the presence of cerium(IV) ammonium sulfate in an acidic medium. The absorbance of the reaction product is measured at the lambdamax, 601 nm. With the same reaction, indapamide is determined by its quenching effect on the fluorescence of excess cerous ions at the emission lambdamax, 350 nm, and the excitation at lambdamax, 300 nm. The reaction conditions were optimized, and Beer's law was obeyed for indapamide at 1.2-9.6 microg/mL with mean recoveries of 99.92 +/- 0.83 and 99.97 +/- 1.11%, respectively. The third method, a stability-indicating densitometric assay, was developed for the determination of indapamide, using toluene-ethyl acetate-glacial acetic acid (69 + 30 + 1, v/v/v) as the developing system and scanning at the lambdamax, 242 nm, in the presence of the degradation product and related substance; for the indapamide concentration range of 0.6-6 microg/spot, the mean recovery was 99.73 +/- 0.71%. The proposed methods were successfully applied to the determination of indapamide in bulk powder and commercial tablets, and the results of the analysis agreed statistically with those obtained with the official method. Furthermore, the methods were validated according to the guidelines of the U.S. Pharmacopeia and also assessed by applying the standard additions technique.

Stability indicating spectrophotometric and spectrodensitometric methods for the determination of diatrizoate sodium in presence of its degradation product

NASA Astrophysics Data System (ADS)

Abd El-Rahman, Mohamed K.; Riad, Safaa M.; Abdel Gawad, Sherif A.; Fawaz, Esraa M.; Shehata, Mostafa A.

2015-02-01

Three sensitive, selective, and precise stability indicating methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA), in the presence of its acidic degradation product (highly cytotoxic 3,5 diamino metabolite) and in pharmaceutical formulation were developed and validated. The first method is a first derivative (D1) spectrophotometric one, which allows the determination of DTA in the presence of its degradate at 231.2 nm (corresponding to zero crossing of the degradate) over a concentration range of 2-24 μg/mL with mean percentage recovery 99.95 ± 0.97%. The second method is the first derivative of the ratio spectra (DD1) by measuring the peak amplitude at 227 nm over the same concentration range as D1 spectrophotometric method, with mean percentage recovery 99.99 ± 1.15%. The third method is a TLC-densitometric one, where DTA was separated from its degradate on silica gel plates using chloroform:methanol:ammonium hydroxide (20:10:2 by volume) as a developing system. This method depends on quantitative densitometric evaluation of thin layer chromatogram of DTA at 238 nm over a concentration range of 4-20 μg/spot, with mean percentage recovery 99.88 ± 0.89%. The selectivity of the proposed methods was tested using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

Novel spectrophotometric determination of chloramphenicol and dexamethasone in the presence of non labeled interfering substances using univariate methods and multivariate regression model updating

NASA Astrophysics Data System (ADS)

Hegazy, Maha A.; Lotfy, Hayam M.; Rezk, Mamdouh R.; Omran, Yasmin Rostom

2015-04-01

Smart and novel spectrophotometric and chemometric methods have been developed and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and dexamethasone sodium phosphate (DSP) in presence of interfering substances without prior separation. The first method depends upon derivative subtraction coupled with constant multiplication. The second one is ratio difference method at optimum wavelengths which were selected after applying derivative transformation method via multiplying by a decoding spectrum in order to cancel the contribution of non labeled interfering substances. The third method relies on partial least squares with regression model updating. They are so simple that they do not require any preliminary separation steps. Accuracy, precision and linearity ranges of these methods were determined. Moreover, specificity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied for analysis of both drugs in their pharmaceutical formulation. The obtained results have been statistically compared to that of an official spectrophotometric method to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision.

Different spectrophotometric methods applied for the analysis of binary mixture of flucloxacillin and amoxicillin: A comparative study.

PubMed

Attia, Khalid A M; Nassar, Mohammed W I; El-Zeiny, Mohamed B; Serag, Ahmed

2016-05-15

Three different spectrophotometric methods were applied for the quantitative analysis of flucloxacillin and amoxicillin in their binary mixture, namely, ratio subtraction, absorbance subtraction and amplitude modulation. A comparative study was done listing the advantages and the disadvantages of each method. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of flucloxacillin and amoxicillin in their binary mixtures. Copyright © 2016 Elsevier B.V. All rights reserved.

New approach for determination of sulfadiazine in pharmaceutical preparations using 4(4-sulphophenylazo)pyrogallol: Kinetic spectrophotometric method.

PubMed

Naser, Naser A; Alasedi, Kasim M; Khan, Zainab A

2018-05-04

A new trend describes the development and validation of a simple, sensitive and selective kinetic spectrophotometric methods for the determination of sulfadiazine in pharmaceutical formulations has been conducted. In this paper, sulfadiazine was derivatized as a new organic compound 4(4-sulphophenylazo) pyrogallol, 4-SPAP, by coupling pyrogallol with diazotized sulfadiazine in medium of controlled pH. 4-SPAP was characterized by techniques of FT-IR, H-NMR, GC-Mass, TG and DSC thermal analysis methods. Solvatochromic behavior in solvents of various polarities was also investigated. The determination of sulfadiazine was accomplished by initial rate and fixed time methods. These methods were based on the reaction of the compound containing sulfadiazine, 4-SPAP, with Ca(II) to form colored product with a maximum absorbance at 520 nm. The two methods were adopted for constructing the calibration curves and examined for their suitability for the quantitation of sulfadiazine in pharmaceuticals. The limit of detection (LOD) and limit of quantification (LOQ) were found to be, by initial rate method, 0.35 and 1.05 μg·mL -1 and that by fixed time method were found to be 0.69 and 2.07 μg·mL -1 , respectively. The percent relative standard deviations (%RSD) for the results ranged from 1.04% to 1.76% and 0.85% to 1.42% for the initial rate and fixed time methods of the proposed kinetic spectrophotometric method, respectively. The existence of common excipients in the pharmaceutical formulation did not produce any significant interference. Statistical comparison was reported as indicated from the F- and t-test data of the proposed methods with that of reference method showing excellent agreement and indicating no significant difference in their accuracy and precision. Copyright © 2018 Elsevier B.V. All rights reserved.

INVESTIGATION AND OPTIMIZATION OF TITRIMETRIC AND SPECTROPHOTOMETRIC METHODS FOR THE ASSAY OF FLUNARIZINE DIHYDROCHLORIDE USING IN SITU BROMINE.

PubMed

Prashanth, Kudige Nagaraj; Swamy, Nagaraju; Basavaiah, Kanakapura

2016-01-01

Three indirect methods for the assay of flunarizine dihydrochloride (FNH) in bulk drug and commercial formulation based on titrimetric and spectrophotometric techniques using bromate-bromide mixture are described. In titrimetry, a measured excess of bromate-bromide mixture is added to an acidified solution of FNH and the unreacted bromine is determined iodometrically (method A). Spectrophotometry involves the addition of a known excess of bromate-bromide mixture to FNH in acid medium followed by estimation of unreacted bromine by its reaction with excess iodide and the liberated iodine (I₃⁻) is either measured at 370 nm (method B) or liberated iodine reacted with starch followed by the measurement of the blue colored starch-iodide complex at 575 run (method C). Titrimetric method is applicable over the range 4.5-30.0 mg FNH (method A), and the reaction stoichiometry is found to be 1:2 (FNH:KBrO₃). The spectrophotometric methods are applicable over the concentration ranges 0.8-16.0 µg/mL and 0.4-8.0 µg/mL FNH for method B and method C, respectively. The molar absorptivities are calculated to be 2.83 x 10⁴ and 4.96 x 10⁴ L mol⁻¹cm⁻¹ for method B and method C, respectively, and the corresponding Sandell sensitivity values are 0.0168 and 0.0096 µg cm⁻². The proposed methods have been applied successfully for the determination of FNH in pure form and in its dosage form and the results were compared with those of a literature method by applying the Student's t-test and F-test.

Spectrophotometric estimation of ambroxol and cetirizine hydrochloride from tablet dosage form.

PubMed

Gowekar, N M; Pande, V V; Kasture, A V; Tekade, A R; Chandorkar, J G

2007-07-01

Fixed dose combination tablets containing ambroxol HCl and cetirizine HCl are clinically used as mucolytic and antiallergic. Several spectrophotometric and HPLC methods have been reported for simultaneous estimation of these drugs with other drugs. The drugs individually and in mixture obeys Beer's law over conc. range 1.2-4.4 microg/mL for cetirizine HCL and for ambroxol HCL 15-52 microg/mL at all five sampling wavelengths (correlation coeff. well above 0.995). The mean recoveries from tablet by standard addition method were 100.18% (+/-2.4) and 100.66 % (+/-2.31). The present work reports simple, accurate and precise spectrophotometric methods for their simultaneous estimation from tablet dosage form.

A novel Raman spectrophotometric method for quantitative measurement of nucleoside triphosphate hydrolysis.

PubMed

Jenkins, R H; Tuma, R; Juuti, J T; Bamford, D H; Thomas, G J

1999-01-01

A novel spectrophotometric method, based upon Raman spectroscopy, has been developed for accurate quantitative determination of nucleoside triphosphate phosphohydrolase (NTPase) activity. The method relies upon simultaneous measurement in real time of the intensities of Raman marker bands diagnostic of the triphosphate (1115 cm(-1)) and diphosphate (1085 cm(-1)) moieties of the NTPase substrate and product, respectively. The reliability of the method is demonstrated for the NTPase-active RNA-packaging enzyme (protein P4) of bacteriophage phi6, for which comparative NTPase activities have been estimated independently by radiolabeling assays. The Raman-determined rate for adenosine triphosphate substrate (8.6 +/- 1.3 micromol x mg(-1) x min(-1) at 40 degrees C) is in good agreement with previous estimates. The versatility of the Raman method is demonstrated by its applicability to a variety of nucleotide substrates of P4, including the natural ribonucleoside triphosphates (ATP, GTP) and dideoxynucleoside triphosphates (ddATP, ddGTP). Advantages of the present protocol include conservative sample requirements (approximately 10(-6) g enzyme/protocol) and relative ease of data collection and analysis. The latter conveniences are particularly advantageous for the measurement of activation energies of phosphohydrolase activity.

Fourth-order derivative spectrophotometric method for simultaneous determination of pseudoephedrine and naproxen in pharmaceutical dosage forms

PubMed Central

Souri, Effat; Mosafer, Amir; Tehrani, Maliheh Barazandeh

2016-01-01

Combination dosage forms of naproxen sodium and pseudoephedrine hydrochloride are used for symptomatic treatment of cold and sinus disorders. In this study, fourth-order derivative spectrophotometric method was used for simultaneous determination of naproxen sodium and pseudoephedrine hydrochloride. The method was linear over the range of 2-28 μg/ml for pseudoephedrine hydrochloride and 4-200 μg/ml for naproxen sodium. The within-day and between-day coefficient of variation values were less than 5.8% and 2.5% for pseudoephedrine hydrochloride and naproxen sodium, respectively. The application of the proposed method for simultaneous determination of naproxen and pseudoephedrine in dosage forms was demonstrated without any special pretreatment. PMID:27168748

Application and validation of superior spectrophotometric methods for simultaneous determination of ternary mixture used for hypertension management.

PubMed

Mohamed, Heba M; Lamie, Nesrine T

2016-02-15

Telmisartan (TL), Hydrochlorothiazide (HZ) and Amlodipine besylate (AM) are co-formulated together for hypertension management. Three smart, specific and precise spectrophotometric methods were applied and validated for simultaneous determination of the three cited drugs. Method A is the ratio isoabsorptive point and ratio difference in subtracted spectra (RIDSS) which is based on dividing the ternary mixture of the studied drugs by the spectrum of AM to get the division spectrum, from which concentration of AM can be obtained by measuring the amplitude values in the plateau region at 360nm. Then the amplitude value of the plateau region was subtracted from the division spectrum and HZ concentration was obtained by measuring the difference in amplitude values at 278.5 and 306nm (corresponding to zero difference of TL) while the total concentration of HZ and TL in the mixture was measured at their isoabsorptive point in the division spectrum at 278.5nm (Aiso). TL concentration is then obtained by subtraction. Method B; double divisor ratio spectra derivative spectrophotometry (RS-DS) and method C; mean centering of ratio spectra (MCR) spectrophotometric methods. The proposed methods did not require any initial separation steps prior the analysis of the three drugs. A comparative study was done between the three methods regarding their; simplicity, sensitivity and limitations. Specificity was investigated by analyzing the synthetic mixtures containing different ratios of the three studied drugs and their tablets dosage form. Statistical comparison of the obtained results with those found by the official methods was done, differences were non-significant in regard to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for TL, HZ and AM. Copyright © 2015 Elsevier B.V. All rights reserved.

Application and validation of superior spectrophotometric methods for simultaneous determination of ternary mixture used for hypertension management

NASA Astrophysics Data System (ADS)

Mohamed, Heba M.; Lamie, Nesrine T.

2016-02-01

Telmisartan (TL), Hydrochlorothiazide (HZ) and Amlodipine besylate (AM) are co-formulated together for hypertension management. Three smart, specific and precise spectrophotometric methods were applied and validated for simultaneous determination of the three cited drugs. Method A is the ratio isoabsorptive point and ratio difference in subtracted spectra (RIDSS) which is based on dividing the ternary mixture of the studied drugs by the spectrum of AM to get the division spectrum, from which concentration of AM can be obtained by measuring the amplitude values in the plateau region at 360 nm. Then the amplitude value of the plateau region was subtracted from the division spectrum and HZ concentration was obtained by measuring the difference in amplitude values at 278.5 and 306 nm (corresponding to zero difference of TL) while the total concentration of HZ and TL in the mixture was measured at their isoabsorptive point in the division spectrum at 278.5 nm (Aiso). TL concentration is then obtained by subtraction. Method B; double divisor ratio spectra derivative spectrophotometry (RS-DS) and method C; mean centering of ratio spectra (MCR) spectrophotometric methods. The proposed methods did not require any initial separation steps prior the analysis of the three drugs. A comparative study was done between the three methods regarding their; simplicity, sensitivity and limitations. Specificity was investigated by analyzing the synthetic mixtures containing different ratios of the three studied drugs and their tablets dosage form. Statistical comparison of the obtained results with those found by the official methods was done, differences were non-significant in regard to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for TL, HZ and AM.

Method and apparatus for producing durationally short ultraviolet or x-ray laser pulses

DOEpatents

MacGowan, B.J.; Matthews, D.L.; Trebes, J.E.

1987-05-05

A method and apparatus is disclosed for producing ultraviolet or x- ray laser pulses of short duration. An ultraviolet or x-ray laser pulse of long duration is progressively refracted, across the surface of an opaque barrier, by a streaming plasma that is produced by illuminating a solid target with a pulse of conventional line focused high power laser radiation. The short pulse of ultraviolet or x-ray laser radiation, which may be amplified to high power, is separated out by passage through a slit aperture in the opaque barrier.

Kinetic spectrophotometric method for trace determination of thiocyanate based on its inhibitory effect

NASA Astrophysics Data System (ADS)

Naik, Radhey M.; Kumar, Basant; Asthana, Abhas

2010-03-01

A kinetic spectrophotometric method for the determination of thiocyanate, based on its inhibitory effect on silver(I) catalyzed substitution of cyanide ion, by phenylhydrazine in hexacyanoferrate(II) is described. Thiocyanate ions form strong complexes with silver(I) catalyst which is used as the basis for its determination at trace level. The progress of reaction was monitored, spectrophotometrically, at 488 nm ( λmax of [Fe(CN) 5PhNHNH 2] 3-, complex) under the optimum reaction conditions at: 2.5 × 10 -3 M [Fe(CN) 6] 4-, 1.0 × 10 -3 M [PhNHNH 2], 8.0 × 10 -7 M [Ag +], pH 2.8 ± 0.02, ionic strength ( μ) 0.02 M (KNO 3) and temperature 30 ± 0.1 °C. A linear relationship obtained between absorbance (measured at 488 nm at different times) and inhibitor concentration, under specified conditions, has been used for the determination of [thiocyanate] in the range of 0.8-8.0 × 10 -8 M with a detection limit of 2 × 10 -9 M. The standard deviation and percentage error have been calculated and reported with each datum. A most plausible mechanistic scheme has been proposed for the reaction. The values of equilibrium constants for complex formation between catalyst-inhibitor ( KCI), catalyst-substrate ( Ks) and Michaelis-Menten constant ( Km) have been computed from the kinetic data. The influence of possible interference by major cations and anions on the determination of thiocyanate and their limits has been investigated.

Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms.

PubMed

Barazandeh Tehrani, Maliheh; Namadchian, Melika; Fadaye Vatan, Sedigheh; Souri, Effat

2013-04-10

A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (1D) 251 nm and (2D) 239 nm and tretinoin at (1D) 364 nm and (2D) 387 nm.The proposed method showed excellent linearity at both first and second derivative order in the range of 60-1200 and 1.25-25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CV<3.81%, error<3.20%). Good agreement between the found andadded concentrations indicates successful application of the proposed method for simultaneous determination of clindamycin and tretinoin in synthetic mixtures and pharmaceutical dosage form.

A nanosilver-based spectrophotometric method for determination of malachite green in surface water samples.

PubMed

Sahraei, R; Farmany, A; Mortazavi, S S; Noorizadeh, H

2013-07-01

A new spectrophotometric method is reported for the determination of nanomolar level of malachite green in surface water samples. The method is based on the catalytic effect of silver nanoparticles on the oxidation of malachite green by hexacyanoferrate (III) in acetate-acetic acid medium. The absorbance is measured at 610 nm with the fixed-time method. Under the optimum conditions, the linear range was 8.0 × 10(-9)-2.0 × 10(-7) mol L(-1) malachite green with a correlation coefficient of 0.996. The limit of detection (S/N = 3) was 2.0 × 10(-9) mol L(-1). Relative standard deviation for ten replicate determinations of 1.0 × 10(-8) mol L(-1) malachite green was 1.86%. The method is featured with good accuracy and reproducibility for malachite green determination in surface water samples without any pre-concentration and separation step.

Determination of cyanide by an indirect spectrophotometric method using 5-Br-PADAP.

PubMed

Fu-Sheng, W; Yu-Qin, L; Fang, Y; Nai-Kui, S

1981-09-01

Complexation of Ni(2+) with cyanide inhibits its colour reaction with 5-Br-PADAP and this reaction is used in the spectrophotometric determination of cyanide at the ug level. Cyanide in industrial waste waters is determined after an initial transfer as hydrogen cyanide from the sample into sodium hydroxide solution with a stream of air.

Development and Validation of New Spectrophotometric Methods to Determine Enrofloxacin in Pharmaceuticals

NASA Astrophysics Data System (ADS)

Rajendraprasad, N.; Basavaiah, K.

2015-07-01

Four spectrophotometric methods, based on oxidation with cerium(IV), are investigated and developed to determine EFX in pure form and in dosage forms. The frst and second methods (Method A and method B) are direct, in which after the oxidation of EFX with cerium(IV) in acid medium, the absorbance of reduced and unreacted oxidant is measured at 275 and 320 nm, respectively. In the third (C) and fourth (D) methods after the reaction between EFX and oxidant is ensured to be completed the surplus oxidant is treated with either N-phenylanthranilic acid (NPA) or Alizarin Red S (ARS) dye and the absorbance of the oxidized NPA or ARS is measured at 440 or 420 nm. The methods showed good linearity over the concentration ranges of 0.5-5.0, 1.25-12.5, 10.0-100.0, and 6.0-60.0 μg/ml, for method A, B, C and D, respectively, with apparent molar absorptivity values of 4.42 × 10 4 , 8.7 × 10 3 , 9.31 × 10 2 , and 2.28 × 10 3 l/(mol· cm). The limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values and other validation results have also been reported. The proposed methods are successfully applied to determine EFX in pure form and in dosage forms.

Stability studies on florfenicol using developed derivative spectrophotometric methods.

PubMed

Elimam, M M; Shantier, S W; Gadkariem, E A; Mohamed, M A; Osman, Z

2017-01-01

This study aims to investigate the stability of florfenicol using previously developed derivative spectrophotometric methods (D 1 and D 2 ). The studied stability-indicating pararmeters included alkali (NaOH, 1M), acid (HCl, 1M), pH changes (buffer pH 2.2-11), temperature (80°C and 100°C at pH 10) and light. A constructed pH profile for the drug degradation rate revealed a significant effect of pH on the drug stability between pH ranges 8 and 11. The obtained profile indicated first order dependence of K obs on [OH - ]. Arrhenius plot at pH 10 was found linear at temperatures 80°C and 100°C with estimated activation energy of 19.35kcal/mol. The calculated rate constant (K obs ), t ½ and t 90 at 25°C were found to be 1.8×10 -3 h, 385h and 58.3h, respectively. The photostability of florfenicol was also studied by exposing the drug solution to direct sunlight during mid-day time. The obtained results reflected the instability of florfenicol under the study conditions. Copyright © 2016 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.

Method and apparatus for producing durationally short ultraviolet or X-ray laser pulses

DOEpatents

MacGowan, Brian J.; Matthews, Dennis L.; Trebes, James E.

1988-01-01

A method and apparatus is disclosed for producing ultraviolet or X-ray laser pulses of short duration (32). An ultraviolet or X-ray laser pulse of long duration (12) is progressively refracted, across the surface of an opaque barrier (28), by a streaming plasma (22) that is produced by illuminating a solid target (16, 18) with a pulse of conventional line focused high power laser radiation (20). The short pulse of ultraviolet or X-ray laser radiation (32), which may be amplified to high power (40, 42), is separated out by passage through a slit aperture (30) in the opaque barrier (28).

Simultaneous determination of a binary mixture of pantoprazole sodium and itopride hydrochloride by four spectrophotometric methods.

PubMed

Ramadan, Nesrin K; El-Ragehy, Nariman A; Ragab, Mona T; El-Zeany, Badr A

2015-02-25

Four simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of a binary mixture containing Pantoprazole Sodium Sesquihydrate (PAN) and Itopride Hydrochloride (ITH). Method (A) is the derivative ratio method ((1)DD), method (B) is the mean centering of ratio spectra method (MCR), method (C) is the ratio difference method (RD) and method (D) is the isoabsorptive point coupled with third derivative method ((3)D). Linear correlation was obtained in range 8-44 μg/mL for PAN by the four proposed methods, 8-40 μg/mL for ITH by methods A, B and C and 10-40 μg/mL for ITH by method D. The suggested methods were validated according to ICH guidelines. The obtained results were statistically compared with those obtained by the official and a reported method for PAN and ITH, respectively, showing no significant difference with respect to accuracy and precision. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous determination of a binary mixture of pantoprazole sodium and itopride hydrochloride by four spectrophotometric methods

NASA Astrophysics Data System (ADS)

Ramadan, Nesrin K.; El-Ragehy, Nariman A.; Ragab, Mona T.; El-Zeany, Badr A.

2015-02-01

Four simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of a binary mixture containing Pantoprazole Sodium Sesquihydrate (PAN) and Itopride Hydrochloride (ITH). Method (A) is the derivative ratio method (1DD), method (B) is the mean centering of ratio spectra method (MCR), method (C) is the ratio difference method (RD) and method (D) is the isoabsorptive point coupled with third derivative method (3D). Linear correlation was obtained in range 8-44 μg/mL for PAN by the four proposed methods, 8-40 μg/mL for ITH by methods A, B and C and 10-40 μg/mL for ITH by method D. The suggested methods were validated according to ICH guidelines. The obtained results were statistically compared with those obtained by the official and a reported method for PAN and ITH, respectively, showing no significant difference with respect to accuracy and precision.

SPECTROPHOTOMETRIC DETERMINATION OF CALCIUM WITH GLYOXAL BIS (2-HYDROXY- ANIL)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Florence, T.M.; Morgan, J.

1961-03-01

A selective method is described for the spectrophotometric determination of calcium using glyoxal bis(2hydroxy-anil) as the chromogenic agent. A comprehensive study of interferences and reagent variables was made. (auth)

Smart stability-indicating spectrophotometric methods for determination of binary mixtures without prior separation.

PubMed

El-Bardicy, Mohammad G; Lotfy, Hayam M; El-Sayed, Mohammad A; El-Tarras, Mohammad F

2008-01-01

Ratio subtraction and isosbestic point methods are 2 innovating spectrophotometric methods used to determine vincamine in the presence of its acid degradation product and a mixture of cinnarizine (CN) and nicergoline (NIC). Linear correlations were obtained in the concentration range from 8-40 microg/mL for vincamine (I), 6-22 microg/mL for CN (II), and 6-36 microg/mL for NIC (III), with mean accuracies 99.72 +/- 0.917% for I, 99.91 +/- 0.703% for II, and 99.58 +/- 0.847 and 99.83 +/- 1.039% for III. The ratio subtraction method was utilized for the analysis of laboratory-prepared mixtures containing different ratios of vincamine and its degradation product, and it was valid in the presence of up to 80% degradation product. CN and NIC in synthetic mixtures were analyzed by the 2 proposed methods with the total content of the mixture determined at their respective isosbestic points of 270.2 and 235.8 nm, and the content of CN was determined by the ratio subtraction method. The proposed method was validated and found to be suitable as a stability-indicating assay method for vincamine in pharmaceutical formulations. The standard addition technique was applied to validate the results and to ensure the specificity of the proposed methods.

Detection of glucose-6-phosphate dehydrogenase deficiency in erythrocytes: a spectrophotometric assay and a fluorescent spot test compared with a cytochemical method.

PubMed

Wolf, B H; Weening, R S; Schutgens, R B; van Noorden, C J; Vogels, I M; Nagelkerke, N J

1987-09-30

The results of a quantitative spectrophotometric enzyme assay, a fluorescent spot test and a cytochemical assay for glucose-6-phosphate dehydrogenase deficiency were compared systematically. The high sensitivity of the spectrophotometric assay and the fluorescent spot test in the detection of severely deficient individuals was confirmed. For the detection of heterozygote females, however both tests were unreliable; the sensitivities of the fluorescent spot test and the spectrophotometric assay being 32% and 11% respectively. Specificities for both tests were high (99%). Introduction of the ratio of glucose-6-phosphate dehydrogenase and pyruvate kinase (G-6-PD/PK ratio) activities increased the sensitivity of the spectrophotometric assay to nearly 100%. It is concluded that the fluorescent spot test should be used for the diagnosis of G-6-PD deficiency in developing countries; whereas if spectrophotometric enzyme assays are available, the G-6-PD/PK ratio should always be performed. In cases where the ratio is less than 0.70, cytochemical analysis is indicated.

Validated spectrophotometric methods for simultaneous determination of Omeprazole, Tinidazole and Doxycycline in their ternary mixture

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Hegazy, Maha A.; Mowaka, Shereen; Mohamed, Ekram Hany

2016-01-01

A comparative study of smart spectrophotometric techniques for the simultaneous determination of Omeprazole (OMP), Tinidazole (TIN) and Doxycycline (DOX) without prior separation steps is developed. These techniques consist of several consecutive steps utilizing zero/or ratio/or derivative spectra. The proposed techniques adopt nine simple different methods, namely direct spectrophotometry, dual wavelength, first derivative-zero crossing, amplitude factor, spectrum subtraction, ratio subtraction, derivative ratio-zero crossing, constant center, and successive derivative ratio method. The calibration graphs are linear over the concentration range of 1-20 μg/mL, 5-40 μg/mL and 2-30 μg/mL for OMP, TIN and DOX, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and successfully applied to commercial pharmaceutical preparation. The methods that are validated according to the ICH guidelines, accuracy, precision, and repeatability, were found to be within the acceptable limits.

Spectrophotometric Method for the Determination of Two Coformulated Drugs with Highly Different Concentrations. Application on Vildagliptin and Metformin Hydrochloride

NASA Astrophysics Data System (ADS)

Zaazaa, H. E.; Elzanfaly, E. S.; Soudi, A. T.; Salem, M. Y.

2016-03-01

A new smart simple validated spectrophotometric method was developed for the determination of two drugs one of which is in a very low concentration compared to the other. The method is based on spiking and dilution then simple mathematical manipulation of the absorbance spectra. This method was applied for the determination of a binary mixture of vildagliptin and metformin hydrochloride in the ratio 50:850 in laboratory prepared mixtures containing both drugs in this ratio and in pharmaceutical dosage form with good recoveries. The developed method was validated according to ICH guidelines and can be used for routine quality control testing.

Three different spectrophotometric methods manipulating ratio spectra for determination of binary mixture of Amlodipine and Atorvastatin

NASA Astrophysics Data System (ADS)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeiny, Badr A.

2011-12-01

Three simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed for the simultaneous determination of Amlodipine besylate (AM) and Atorvastatin calcium (AT) in tablet dosage forms. The first method is first derivative of the ratio spectra ( 1DD), the second is ratio subtraction and the third is the method of mean centering of ratio spectra. The calibration curve is linear over the concentration range of 3-40 and 8-32 μg/ml for AM and AT, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and they are applied to commercial pharmaceutical preparation of the subjected drugs. Standard deviation is <1.5 in the assay of raw materials and tablets. Methods are validated as per ICH guidelines and accuracy, precision, repeatability and robustness are found to be within the acceptable limit.

Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms

PubMed Central

2013-01-01

A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (1D) 251 nm and (2D) 239 nm and tretinoin at (1D) 364 nm and (2D) 387 nm. The proposed method showed excellent linearity at both first and second derivative order in the range of 60–1200 and 1.25–25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CV<3.81%, error<3.20%). Good agreement between the found and added concentrations indicates successful application of the proposed method for simultaneous determination of clindamycin and tretinoin in synthetic mixtures and pharmaceutical dosage form. PMID:23575006

Spectrophotometric Methods for the Determination of Sitagliptin and Vildagliptin in Bulk and Dosage Forms

PubMed Central

El-Bagary, Ramzia I.; Elkady, Ehab F.; Ayoub, Bassam M.

2011-01-01

Simple, accurate and precise spectrophotometric methods have been developed for the determination of sitagliptin and vildagliptin in bulk and dosage forms. The proposed methods are based on the charge transfer complexes of sitagliptin phosphate and vildagliptin with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetrachloro-1,4-benzoquinone (p-chloranil). All the variables were studied to optimize the reactions conditions. For sitagliptin, Beer’s law was obeyed in the concentration ranges of 50-300 μg/ml, 20-120 μg/ml and 100-900 μg/ml with DDQ, TCNQ and p-chloranil, respectively. For vildagliptin, Beer’s law was obeyed in the concentration ranges of 50-300 μg/ml, 10-85 μg/ml and 50-350 μg/ml with DDQ, TCNQ and p-chloranil, respectively. The developed methods were validated and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms. PMID:23675221

Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form

NASA Astrophysics Data System (ADS)

Khattab, Fatma I.; Ramadan, Nesrin K.; Hegazy, Maha A.; Al-Ghobashy, Medhat A.; Ghoniem, Nermine S.

2015-03-01

Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D1) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD1) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D1 at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL-1 and 0.5-10.0 μg mL-1 for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method.

Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form.

PubMed

Khattab, Fatma I; Ramadan, Nesrin K; Hegazy, Maha A; Al-Ghobashy, Medhat A; Ghoniem, Nermine S

2015-03-15

Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D(1)) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD(1)) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D(1) at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL(-1) and 0.5-10.0 μg mL(-1) for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method. Copyright © 2015 Elsevier B.V. All rights reserved.

Spectrophotometric and HPLC determinations of anti-diabetic drugs, rosiglitazone maleate and metformin hydrochloride, in pure form and in pharmaceutical preparations.

PubMed

Onal, Armağan

2009-12-01

In this study, three spectrophotometric methods and one HPLC method were developed for analysis of anti-diabetic drugs in tablets. The two spectrophotometric methods were based on the reaction of rosiglitazone (RSG) with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and bromocresol green (BCG). Linear relationship between the absorbance at lambda(max) and the drug concentration was found to be in the ranges 6.0-50.0 and 1.5-12 microg ml(-1) for DDQ and BCG methods, respectively. The third spectrophotometric method consists of a zero-crossing first-derivative spectrophotometric method for simultaneous analysis of RSG and metformin (MTF) in tablets. The calibration curves were linear within the concentration ranges of 5.0-50 microg ml(-1) for RSG and 1.0-10.0 microg ml(-1) for MTF. The fourth method is a rapid stability-indicating HPLC method developed for the determination of RSG. A linear response was observed within the concentration range of 0.25-2.5 microg ml(-1). The proposed methods have been successfully applied to the tablet analysis.

Different Spectrophotometric Methods for Simultaneous Determination of Trelagliptin and Its Acid Degradation Product.

PubMed

Mowaka, Shereen; Ayoub, Bassam M; Hassan, Mostafa A; Zaghary, Wafaa A

2018-01-01

New spectrophotometric and chemometric methods were carried out for the simultaneous assay of trelagliptin (TRG) and its acid degradation product (TAD) and applied successfully as a stability indicating assay to recently approved Zafatek® tablets. TAD was monitored using TLC to ensure complete degradation. Furthermore, HPLC was used to confirm dealing with one major acid degradation product. The proposed methods were developed by manipulating zero-order, first-derivative, and ratio spectra of TRG and TAD using simultaneous equation, first-derivative, and mean-centering methods, respectively. Using Spectra Manager II and Minitab v.14 software, the absorbance at 274 nm-260.4 nm, amplitudes at 260.4 nm-274.0 nm, and mean-centered values at 287.6 nm-257.2 nm were measured against methanol as a blank for TRG and TAD, respectively. Linearity and the other validation parameters were acceptable at concentration ranges of 5-50  μ g/mL and 2.5-25  μ g/mL for TRG and TAD, respectively. Using one-way analysis of variance (ANOVA), the optimized methods were compared and proved to be accurate for the simultaneous assay of TRG and TAD.

A simple spectrophotometric method for the determination of beta-blockers in dosage forms.

PubMed

Al-Ghannam, S M

2006-01-23

A simple, extraction-free spectrophotometric method is proposed for the analysis of some beta-blockers, namely atenolol, timolol and nadolol. The method is based on the interaction of the drugs in chloroform with 0.1% chloroformic solutions of acidic sulphophthalein dyes to form stable, yellow-coloured, ion-pair complexes peaking at 415 nm. The dyes used were bromophenol blue (BPB), bromothymol blue (BTB) and bromocresol purple (BCP). Under the optimum conditions, the three drugs could be assayed in the concentration range 1-10 microg ml(-1) with correlation coefficient (n = 5) more than 0.999 in all cases. The stoichiometry of the reaction was found to be 1:1 in all cases and the conditional stability constant (K(F)) of the complexes have been calculated. The free energy changes (DeltaG) were determined for all complexes formed. The interference likely to be introduced from co-formulated drugs was studied and their tolerance limits were determined. The proposed method was then applied to dosage-forms the percentage recoveries ranges from 99.12-100.95, and the results obtained were compared favorably with those given with the official methods.

Determination of Trace Amounts of Lead Using the Flotation-spectrophotometric method

PubMed Central

Shiri, Sabah; Delpisheh, Ali; Haeri, Ali; Poornajaf, Abdolhossein; Golzadeh, Babak; Shiri, Sina

2011-01-01

The present study describes a simple and highly selective method for separation, preconcentration and spectrophotometric determination of extremely low concentrations of lead. It is based on flotation of a complex of Pb2+ ions and Alizarin yellow between aqueous and n-hexane interface at pH = 6. The proposed procedure is also applied for determination of lead in both tap water and prepared sea water samples. Beer’s Law was obeyed over the concentration range of 3.86 × 10–8 To 8.20 × 10–7 molL−1 (8–170 ngmL−1) with an apparent molar absorptivity of 1.33 × 106 molL−1 cm−1 for a 100 mL aliquot of the water sample. The detection limit (n = 10) was 8.7 × 10–9 molL−1 (1.0 ngmL−1) and the Relative standard deviation (R.S.D), (n = 10) for 7.2 × 10–7 molL−1 (150 ngmL−1) of Pb (II) was 4.36%. A notable advantage of the method is that the determination of Pb (II) is free from the interference of almost all cations and ions found in the environment and waste water samples. The determination of Pb (II) in tap and synthetic seawater samples was also carried out by the present method. The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples.

Determination of Trace Amounts of Lead Using the Flotation-spectrophotometric method

PubMed Central

Shiri, Sabah; Delpisheh, Ali; Haeri, Ali; Poornajaf, Abdolhossein; Golzadeh, Babak; Shiri, Sina

2010-01-01

The present study describes a simple and highly selective method for separation, preconcentration and spectrophotometric determination of extremely low concentrations of lead. It is based on flotation of a complex of Pb2+ ions and Alizarin yellow between aqueous and n-hexane interface at pH = 6. The proposed procedure is also applied for determination of lead in both tap water and prepared sea water samples. Beer’s Law was obeyed over the concentration range of 3.86 × 10−8 To 8.20 × 10−7 molL−1 (8–170 ngmL−1) with an apparent molar absorptivity of 1.33 × 106 molL−1 cm−1 for a 100 mL aliquot of the water sample. The detection limit (n = 10) was 8.7 × 10−9 molL−1 (1.0 ngmL−1) and the Relative standard deviation (R.S.D), (n = 10) for 7.2 × 10−7 molL−1 (150 ngmL−1) of Pb (II) was 4.36%. A notable advantage of the method is that the determination of Pb (II) is free from the interference of almost all cations and ions found in the environment and waste water samples. The determination of Pb (II) in tap and synthetic seawater samples was also carried out by the present method. The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples. PMID:21234287

Fine structural dependence of ultraviolet reflections in the King Penguin beak horn.

PubMed

Dresp, Birgitta; Langley, Keith

2006-03-01

The visual perception of many birds extends into the near-ultraviolet (UV) spectrum and ultraviolet is used by some to communicate. The beak horn of the King Penguin (Aptenodytes patagonicus) intensely reflects in the ultraviolet and this appears to be implicated in partner choice. In a preliminary study, we recently demonstrated that this ultraviolet reflectance has a structural basis, resulting from crystal-like photonic structures, capable of reflecting in the near-UV. The present study attempted to define the origin of the photonic elements that produce the UV reflectance and to better understand how the UV signal is optimized by their fine structure. Using light and electron microscopic analysis combined with new spectrophotometric data, we describe here in detail the fine structure of the entire King Penguin beak horn in addition to that of its photonic crystals. The data obtained reveal a one-dimensional structural periodicity within this tissue and demonstrate a direct relationship between its fine structure and its function. In addition, they suggest how the photonic structures are produced and how they are stabilized. The measured lattice dimensions of the photonic crystals, together with morphological data on its composition, permit predictions of the wavelength of reflected light. These correlate well with experimentally observed values. The way the UV signal is optimized by the fine structure of the beak tissue is discussed with regard to its putative biological role.

Mean centering of double divisor ratio spectra, a novel spectrophotometric method for analysis of ternary mixtures

NASA Astrophysics Data System (ADS)

Hassan, Said A.; Elzanfaly, Eman S.; Salem, Maissa Y.; El-Zeany, Badr A.

2016-01-01

A novel spectrophotometric method was developed for determination of ternary mixtures without previous separation, showing significant advantages over conventional methods. The new method is based on mean centering of double divisor ratio spectra. The mathematical explanation of the procedure is illustrated. The method was evaluated by determination of model ternary mixture and by the determination of Amlodipine (AML), Aliskiren (ALI) and Hydrochlorothiazide (HCT) in laboratory prepared mixtures and in a commercial pharmaceutical preparation. For proper presentation of the advantages and applicability of the new method, a comparative study was established between the new mean centering of double divisor ratio spectra (MCDD) and two similar methods used for analysis of ternary mixtures, namely mean centering (MC) and double divisor of ratio spectra-derivative spectrophotometry (DDRS-DS). The method was also compared with a reported one for analysis of the pharmaceutical preparation. The method was validated according to the ICH guidelines and accuracy, precision, repeatability and robustness were found to be within the acceptable limits.

Novel spectrophotometric method for determination of cinacalcet hydrochloride in its tablets via derivatization with 1,2-naphthoquinone-4-sulphonate

PubMed Central

2012-01-01

This study represents the first report on the development of a novel spectrophotometric method for determination of cinacalcet hydrochloride (CIN) in its tablet dosage forms. Studies were carried out to investigate the reaction between CIN and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. In alkaline medium (pH 8.5), an orange red-colored product exhibiting maximum absorption peak (λmax) at 490 nm was produced. The stoichiometry and kinetic of the reaction were investigated and the reaction mechanism was postulated. This color-developing reaction was employed in the development of a simple and rapid visible-spectrophotometric method for determination of CIN in its tablets. Under the optimized reaction conditions, Beer's law correlating the absorbance with CIN concentration was obeyed in the range of 3 - 100 μg/ml with good correlation coefficient (0.9993). The molar absorptivity (ε) was 4.2 × 105 l/mol/cm. The limits of detection and quantification were 1.9 and 5.7 μg/ml, respectively. The precision of the method was satisfactory; the values of relative standard deviations (RSD) did not exceed 2%. No interference was observed from the excipients that are present in the tablets. The proposed method was applied successfully for the determination of CIN in its pharmaceutical tablets with good accuracy and precisions; the label claim percentage was 100.80 - 102.23 ± 1.27 - 1.62%. The results were compared favorably with those of a reference pre-validated method. The method is practical and valuable in terms of its routine application in quality control laboratories. PMID:22305461

Highly sensitive catalytic spectrophotometric determination of ruthenium

NASA Astrophysics Data System (ADS)

Naik, Radhey M.; Srivastava, Abhishek; Prasad, Surendra

2008-01-01

A new and highly sensitive catalytic kinetic method (CKM) for the determination of ruthenium(III) has been established based on its catalytic effect on the oxidation of L-phenylalanine ( L-Pheala) by KMnO 4 in highly alkaline medium. The reaction has been followed spectrophotometrically by measuring the decrease in the absorbance at 526 nm. The proposed CKM is based on the fixed time procedure under optimum reaction conditions. It relies on the linear relationship where the change in the absorbance (Δ At) versus added Ru(III) amounts in the range of 0.101-2.526 ng ml -1 is plotted. Under the optimum conditions, the sensitivity of the proposed method, i.e. the limit of detection corresponding to 5 min is 0.08 ng ml -1, and decreases with increased time of analysis. The method is featured with good accuracy and reproducibility for ruthenium(III) determination. The ruthenium(III) has also been determined in presence of several interfering and non-interfering cations, anions and polyaminocarboxylates. No foreign ions interfered in the determination ruthenium(III) up to 20-fold higher concentration of foreign ions. In addition to standard solutions analysis, this method was successfully applied for the quantitative determination of ruthenium(III) in drinking water samples. The method is highly sensitive, selective and very stable. A review of recently published catalytic spectrophotometric methods for the determination of ruthenium(III) has also been presented for comparison.

Development and Validation of an Extractive Spectrophotometric Method for Miconazole Nitrate Assay in Pharmaceutical Formulations.

PubMed

Eticha, Tadele; Kahsay, Getu; Hailu, Teklebrhan; Gebretsadikan, Tesfamichael; Asefa, Fitsum; Gebretsadik, Hailekiros; Thangabalan, Boovizhikannan

2018-01-01

A simple extractive spectrophotometric technique has been developed and validated for the determination of miconazole nitrate in pure and pharmaceutical formulations. The method is based on the formation of a chloroform-soluble ion-pair complex between the drug and bromocresol green (BCG) dye in an acidic medium. The complex showed absorption maxima at 422 nm, and the system obeys Beer's law in the concentration range of 1-30  µ g/mL with molar absorptivity of 2.285 × 10 4  L/mol/cm. The composition of the complex was studied by Job's method of continuous variation, and the results revealed that the mole ratio of drug : BCG is 1 : 1. Full factorial design was used to optimize the effect of variable factors, and the method was validated based on the ICH guidelines. The method was applied for the determination of miconazole nitrate in real samples.

Method for the detection of nitro-containing compositions using ultraviolet photolysis

DOEpatents

Reagen, William K.; Lancaster, Gregory D.; Partin, Judy K.; Moore, Glenn A.

2000-01-01

A method for detecting nitro-containing compositions (e.g. nitrate/nitrite materials) in water samples and on solid substrates. In a water sample, ultraviolet light is applied to the sample so that dissolved nitro compositions therein will photolytically dissociate into gaseous nitrogen oxides (NO.sub.2(g) and/or NO.sub.(g)). A carrier gas is then introduced into the sample to generate a gaseous stream which includes the carrier gas combined with any gaseous nitrogen oxides. The carrier gas is thereafter directed into a detector. To detect nitro-compositions on solid substrates, ultraviolet light is applied thereto. A detector is then used to detect any gaseous nitrogen oxides which are photolytically generated during ultraviolet illumination. An optional carrier gas may be applied to the substrate during illumination to produce a gaseous stream which includes the carrier gas and any gaseous nitrogen oxides. The gaseous stream is then supplied to the detector.

Advanced spectrophotometric chemometric methods for resolving the binary mixture of doxylamine succinate and pyridoxine hydrochloride.

PubMed

Katsarov, Plamen; Gergov, Georgi; Alin, Aylin; Pilicheva, Bissera; Al-Degs, Yahya; Simeonov, Vasil; Kassarova, Margarita

2018-03-01

The prediction power of partial least squares (PLS) and multivariate curve resolution-alternating least squares (MCR-ALS) methods have been studied for simultaneous quantitative analysis of the binary drug combination - doxylamine succinate and pyridoxine hydrochloride. Analysis of first-order UV overlapped spectra was performed using different PLS models - classical PLS1 and PLS2 as well as partial robust M-regression (PRM). These linear models were compared to MCR-ALS with equality and correlation constraints (MCR-ALS-CC). All techniques operated within the full spectral region and extracted maximum information for the drugs analysed. The developed chemometric methods were validated on external sample sets and were applied to the analyses of pharmaceutical formulations. The obtained statistical parameters were satisfactory for calibration and validation sets. All developed methods can be successfully applied for simultaneous spectrophotometric determination of doxylamine and pyridoxine both in laboratory-prepared mixtures and commercial dosage forms.

Methods of automatic nucleotide-sequence analysis. Multicomponent spectrophotometric analysis of mixtures of nucleic acid components by a least-squares procedure

PubMed Central

Lee, Sheila; McMullen, D.; Brown, G. L.; Stokes, A. R.

1965-01-01

1. A theoretical analysis of the errors in multicomponent spectrophotometric analysis of nucleoside mixtures, by a least-squares procedure, has been made to obtain an expression for the error coefficient, relating the error in calculated concentration to the error in extinction measurements. 2. The error coefficients, which depend only on the `library' of spectra used to fit the experimental curves, have been computed for a number of `libraries' containing the following nucleosides found in s-RNA: adenosine, guanosine, cytidine, uridine, 5-ribosyluracil, 7-methylguanosine, 6-dimethylaminopurine riboside, 6-methylaminopurine riboside and thymine riboside. 3. The error coefficients have been used to determine the best conditions for maximum accuracy in the determination of the compositions of nucleoside mixtures. 4. Experimental determinations of the compositions of nucleoside mixtures have been made and the errors found to be consistent with those predicted by the theoretical analysis. 5. It has been demonstrated that, with certain precautions, the multicomponent spectrophotometric method described is suitable as a basis for automatic nucleotide-composition analysis of oligonucleotides containing nine nucleotides. Used in conjunction with continuous chromatography and flow chemical techniques, this method can be applied to the study of the sequence of s-RNA. PMID:14346087

Method for plasma formation for extreme ultraviolet lithography-theta pinch

DOEpatents

Hassanein, Ahmed [Naperville, IL; Konkashbaev, Isak [Bolingbrook, IL; Rice, Bryan [Hillsboro, OR

2007-02-20

A device and method for generating extremely short-wave ultraviolet electromagnetic wave, utilizing a theta pinch plasma generator to produce electromagnetic radiation in the range of 10 to 20 nm. The device comprises an axially aligned open-ended pinch chamber defining a plasma zone adapted to contain a plasma generating gas within the plasma zone; a means for generating a magnetic field radially outward of the open-ended pinch chamber to produce a discharge plasma from the plasma generating gas, thereby producing a electromagnetic wave in the extreme ultraviolet range; a collecting means in optical communication with the pinch chamber to collect the electromagnetic radiation; and focusing means in optical communication with the collecting means to concentrate the electromagnetic radiation.

Kinetic spectrophotometric method for determination of amlodipine besylate in its pharmaceutical tablets

PubMed Central

Mahmoud, Ashraf M.; Abdel-Wadood, Hanaa M.; Mohamed, Niveen A.

2012-01-01

A simple and sensitive kinetic spectrophotometric method has been developed and validated for determination of amlodipine besylate (AML). The method was based on the condensation reaction of AML with 7-chloro-4-nitro-2,1,3-benzoxadiazole in an alkaline buffer (pH 8.6) producing a highly colored product. The color development was monitored spectrophometrically at the maximum absorption λmax 470 nm. The factors affecting the reaction were studied and the conditions were optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. Moreover, both the activation energy and the specific rate constant (at 70 °C) of the reaction were found to be 6.74 kcal mole−1 and 3.58 s−1, respectively. The initial rate and fixed time methods were utilized for constructing the calibration graphs for the determination of AML concentration. Under the optimum reaction conditions, the limits of detection and quantification were 0.35 and 1.05 μg/mL, respectively. The precision of the method was satisfactory; the relative standard deviations were 0.85–1.76%. The proposed method was successfully applied to the analysis of AML in its pure form and tablets with good accuracy; the recovery percentages ranged from 99.55±1.69% to 100.65±1.48%. The results were compared with that of the reported method. PMID:29403763

A comparative study of progressive versus successive spectrophotometric resolution techniques applied for pharmaceutical ternary mixtures

NASA Astrophysics Data System (ADS)

Saleh, Sarah S.; Lotfy, Hayam M.; Hassan, Nagiba Y.; Salem, Hesham

2014-11-01

This work represents a comparative study of a novel progressive spectrophotometric resolution technique namely, amplitude center method (ACM), versus the well-established successive spectrophotometric resolution techniques namely; successive derivative subtraction (SDS); successive derivative of ratio spectra (SDR) and mean centering of ratio spectra (MCR). All the proposed spectrophotometric techniques consist of several consecutive steps utilizing ratio and/or derivative spectra. The novel amplitude center method (ACM) can be used for the determination of ternary mixtures using single divisor where the concentrations of the components are determined through progressive manipulation performed on the same ratio spectrum. Those methods were applied for the analysis of the ternary mixture of chloramphenicol (CHL), dexamethasone sodium phosphate (DXM) and tetryzoline hydrochloride (TZH) in eye drops in the presence of benzalkonium chloride as a preservative. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs. The proposed methods were validated according to the ICH guidelines. A comparative study was conducted between those methods regarding simplicity, limitation and sensitivity. The obtained results were statistically compared with those obtained from the official BP methods, showing no significant difference with respect to accuracy and precision.

Incipient fault diagnosis of power transformers using optical spectro-photometric technique

NASA Astrophysics Data System (ADS)

Hussain, K.; Karmakar, Subrata

2015-06-01

Power transformers are the vital equipment in the network of power generation, transmission and distribution. Mineral oil in oil-filled transformers plays very important role as far as electrical insulation for the winding and cooling of the transformer is concerned. As transformers are always under the influence of electrical and thermal stresses, incipient faults like partial discharge, sparking and arcing take place. As a result, mineral oil deteriorates there by premature failure of the transformer occurs causing huge losses in terms of revenue and assets. Therefore, the transformer health condition has to be monitored continuously. The Dissolved Gas Analysis (DGA) is being extensively used for this purpose, but it has some drawbacks like it needs carrier gas, regular instrument calibration, etc. To overcome these drawbacks, Ultraviolet (UV) -Visible and Fourier Transform Infrared (FTIR) Spectro-photometric techniques are used as diagnostic tools for investigating the degraded transformer oil affected by electrical, mechanical and thermal stresses. The technique has several advantages over the conventional DGA technique.

Comparative study on the selectivity of various spectrophotometric techniques for the determination of binary mixture of fenbendazole and rafoxanide.

PubMed

Saad, Ahmed S; Attia, Ali K; Alaraki, Manal S; Elzanfaly, Eman S

2015-11-05

Five different spectrophotometric methods were applied for simultaneous determination of fenbendazole and rafoxanide in their binary mixture; namely first derivative, derivative ratio, ratio difference, dual wavelength and H-point standard addition spectrophotometric methods. Different factors affecting each of the applied spectrophotometric methods were studied and the selectivity of the applied methods was compared. The applied methods were validated as per the ICH guidelines and good accuracy; specificity and precision were proven within the concentration range of 5-50 μg/mL for both drugs. Statistical analysis using one-way ANOVA proved no significant differences among the proposed methods for the determination of the two drugs. The proposed methods successfully determined both drugs in laboratory prepared and commercially available binary mixtures, and were found applicable for the routine analysis in quality control laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Tolerance of an albino fish to ultraviolet-B radiation

USGS Publications Warehouse

Fabacher, David L.; Little, Edward E.; Ostrander, Gary K.

1999-01-01

We exposed albino and pigmented medakaOryzias latipes to simulated solar ultraviolet-B (UVB) radiation to determine if albino medaka were less tolerant of UVB radiation than medaka pigmented with melanin. There was no difference in the number of albino and pigmented medaka that died during the exposure period. Spectrophotometric analyses of the outer dorsal skin layers from albino and pigmented medaka indicated that, prior to exposure, both groups of fish had similar amounts of an apparent colorless non-melanin photoprotective substance that appears to protect other fish species from UVB radiation. Our results indicate that albino medaka were as tolerant of UVB radiation as pigmented medaka because they had similar amounts of this photoprotective substance in the outer layers of the skin.

New Sensitive Kinetic Spectrophotometric Methods for Determination of Omeprazole in Dosage Forms

PubMed Central

Mahmoud, Ashraf M.

2009-01-01

New rapid, sensitive, and accurate kinetic spectrophotometric methods were developed, for the first time, to determine omeprazole (OMZ) in its dosage forms. The methods were based on the formation of charge-transfer complexes with both iodine and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The variables that affected the reactions were carefully studied and optimized. The formed complexes and the site of interaction were examined by UV/VIS, IR, and 1H-NMR techniques, and computational molecular modeling. Under optimum conditions, the stoichiometry of the reactions between OMZ and the acceptors was found to be 1 : 1. The order of the reactions and the specific rate constants were determined. The thermodynamics of the complexes were computed and the mechanism of the reactions was postulated. The initial rate and fixed time methods were utilized for the determination of OMZ concentrations. The linear ranges for the proposed methods were 0.10–3.00 and 0.50–25.00 μg mL−1 with the lowest LOD of 0.03 and 0.14 μg mL−1 for iodine and DDQ, respectively. Analytical performance of the methods was statistically validated; RSD was <1.25% for the precision and <1.95% for the accuracy. The proposed methods were successfully applied to the analysis of OMZ in its dosage forms; the recovery was 98.91–100.32% ± 0.94–1.84, and was found to be comparable with that of reference method. PMID:20140076

Comparison of Spectrophotometric and Visual Readings of NCCLS Method and Evaluation of a Colorimetric Method Based on Reduction of a Soluble Tetrazolium Salt, 2,3-Bis {2-Methoxy-4-Nitro-5-[(Sulfenylamino) Carbonyl]-2H- Tetrazolium-Hydroxide}, for Antifungal Susceptibility Testing of Aspergillus Species

PubMed Central

Meletiadis, Joseph; Mouton, Johan W.; Meis, Jacques F. G. M.; Bouman, Bianca A.; Donnelly, Peter J.; Verweij, Paul E.

2001-01-01

The susceptibilities of 25 clinical isolates of various Aspergillus species (Aspergillus fumigatus, A. flavus, A. terreus, A. ustus, and A. nidulans) to itraconazole (ITC) and amphotericin B (AMB) were determined using the standard proposed by NCCLS for antifungal susceptibility testing of filamentous fungi, a modification of this method using spectrophotometric readings, and a colorimetric method using the tetrazolium salt 2,3-bis {2-methoxy-4-nitro-5-[(sulfenylamino) carbonyl]-2H-tetrazolium-hydroxide} (XTT). Five MIC end points for ITC (MIC-0, no visible growth or ≤5% the growth control value [GC]; MIC-1, slight growth or 6 to 25% the GC; MIC-2, prominent reduction in growth or 26 to 50% the GC; MIC-3, slight reduction in growth or 51 to 75% the GC; and MIC-4, no reduction in growth or 76 to 100% the GC) and one for AMB (MIC-0) were determined visually by four observers and spectrophotometrically. The intraexperimental (between the observers) and interexperimental (between the experiments) levels of agreement of the NCCLS and XTT methods exceeded 95% for MIC-0 of AMB and MIC-0 and MIC-1 of ITC. The MIC-2 of ITC showed lower reproducibility, although spectrophotometric reading and/or incubation for 48 h increased the interexperimental reproducibility from 85 to >93%. Between visual and spectrophotometric readings, high levels of agreement were found for AMB (≈97%) and MIC-1 (≈92%) and MIC-2 (≈88%) of ITC. Poor agreement was found for MIC-0 of ITC (51% after 24 h), since the spectrophotometric readings resulted in higher MIC-0 values than the visual readings. The agreement was increased to 98% by shifting the threshold level of MIC-0 from 5 to 10% relative optical density and by establishing an optical density of greater than 0.1 for the GC as the validation criterion. No statistically significant differences were found between the NCCLS method and the XTT method, with the levels of agreement exceeding 97% for MIC-0 of AMB and 83% for MIC-0, MIC-1, and MIC

A highly sensitive kinetic spectrophotometric method for the determination of ascorbic Acid in pharmaceutical samples.

PubMed

Shishehbore, Masoud Reza; Aghamiri, Zahra

2014-01-01

In this study, a new reaction system for quantitative determination of ascorbic acid was introduced. The developed method is based on inhibitory effect of ascorbic acid on the Orange G-bromate system. The change in absorbance was followed spectrophotometrically at 478 nm. The dependence of sensitivity on the reaction variables including reagents concentration, temperature and time was investigated. Under optimum experimental conditions, calibration curve was linear over the range 0.7 - 33.5 μg mL(-1) of ascorbic acid including two linear segments and the relative standard deviations (n = 6) for 5.0 and 20.0 μg mL(-1) of ascorbic acid were 1.08 and 1.02%, respectively. The limit of detection was 0.21 μg mL(-) (1) of ascorbic acid. The effect of diverse species was also investigated. The developed method was successfully applied for the determination of ascorbic acid in pharmaceutical samples. The results were in a good agreement with those of reference method.

Pinaverium Bromide: Development and Validation of Spectrophotometric Methods for Assay and Dissolution Studies.

PubMed

Martins, Danielly da Fonte Carvalho; Florindo, Lorena Coimbra; Machado, Anna Karolina Mouzer da Silva; Todeschini, Vítor; Sangoi, Maximiliano da Silva

2017-11-01

This study presents the development and validation of UV spectrophotometric methods for the determination of pinaverium bromide (PB) in tablet assay and dissolution studies. The methods were satisfactorily validated according to International Conference on Harmonization guidelines. The response was linear (r2 > 0.99) in the concentration ranges of 2-14 μg/mL at 213 nm and 10-70 μg/mL at 243 nm. The LOD and LOQ were 0.39 and 1.31 μg/mL, respectively, at 213 nm. For the 243 nm method, the LOD and LOQ were 2.93 and 9.77 μg/mL, respectively. Precision was evaluated by RSD, and the obtained results were lower than 2%. Adequate accuracy was also obtained. The methods proved to be robust using a full factorial design evaluation. For PB dissolution studies, the best conditions were achieved using a United States Pharmacopeia Dissolution Apparatus 2 (paddle) at 50 rpm and with 900 mL 0.1 M hydrochloric acid as the dissolution medium, presenting satisfactory results during the validation tests. In addition, the kinetic parameters of drug release were investigated using model-dependent methods, and the dissolution profiles were best described by the first-order model. Therefore, the proposed methods were successfully applied for the assay and dissolution analysis of PB in commercial tablets.

Different Spectrophotometric Methods for Simultaneous Determination of Trelagliptin and Its Acid Degradation Product

PubMed Central

Hassan, Mostafa A.; Zaghary, Wafaa A.

2018-01-01

New spectrophotometric and chemometric methods were carried out for the simultaneous assay of trelagliptin (TRG) and its acid degradation product (TAD) and applied successfully as a stability indicating assay to recently approved Zafatek® tablets. TAD was monitored using TLC to ensure complete degradation. Furthermore, HPLC was used to confirm dealing with one major acid degradation product. The proposed methods were developed by manipulating zero-order, first-derivative, and ratio spectra of TRG and TAD using simultaneous equation, first-derivative, and mean-centering methods, respectively. Using Spectra Manager II and Minitab v.14 software, the absorbance at 274 nm–260.4 nm, amplitudes at 260.4 nm–274.0 nm, and mean-centered values at 287.6 nm–257.2 nm were measured against methanol as a blank for TRG and TAD, respectively. Linearity and the other validation parameters were acceptable at concentration ranges of 5–50 μg/mL and 2.5–25 μg/mL for TRG and TAD, respectively. Using one-way analysis of variance (ANOVA), the optimized methods were compared and proved to be accurate for the simultaneous assay of TRG and TAD. PMID:29629213

Spectrophotometric and Spectrofluorimetric Studies on Azilsartan Medoxomil and Chlorthalidone to Be Utilized in Their Determination in Pharmaceuticals

PubMed Central

Ebeid, Walid M; Elkady, Ehab F; El-Zaher, Asmaa A; El-Bagary, Ramzia I; Patonay, Gabor

2014-01-01

The recently approved angiotensin II receptor blocker, azilsartan medoxomil (AZL), was determined spectrophotometrically and spectrofluorimetrically in its combination with chlorthalidone (CLT) in their combined dosage form. The UV-spectrophotometric technique depends on simultaneous measurement of the first derivative spectra for AZL and CLT at 286 and 257 nm, respectively, in methanol. The spectrofluorimetric technique depends on measurement of the fourth derivative of the synchronous spectra intensities of AZL in presence of CLT at 298 nm in methanol. The effects of different solvents on spectrophotometric and spectrofluorimetric responses were studied. For, the spectrofluorimetric study, the effect of pH and micelle-assisted fluorescence enhancement were also studied. Linearity, accuracy, and precision were found to be satisfactory over the concentration ranges of 8–50 μg mL−1 and 2–20 μg mL−1 for AZL and CLT, respectively, in the spectrophotometric method as well as 0.01–0.08 μg mL−1 for AZL in the spectrofluorimetric method. The methods were successfully applied for the determination of the studied drugs in their co-formulated tablets. The developed methods are inexpensive and simple for the quality control and routine analysis of the cited drugs in bulk and in pharmaceuticals. PMID:24855334

[Spectrophotometric determination of prodigiozan in ampule solutions].

PubMed

Shchedrina, L E; Brutko, L I; Rastunova, G A; Shcherbakova, E G

1984-06-01

Based on a study of the absorption properties of prodigiosan it has been shown that its UV absorption spectrum is characterized by an arm at 250-260 nm with an inflection point at 260 nm. The concentration ranges within which the optical density of prodigiosan solution obeyed the Bouguer-Lambert-Beer law were measured. This allowed the development of a quantitative spectrophotometric method for determination of prodigiosan in ampouled solutions.

Analysis of Closely Related Antioxidant Nutraceuticals Using the Green Analytical Methodology of ANN and Smart Spectrophotometric Methods.

PubMed

Korany, Mohamed A; Gazy, Azza A; Khamis, Essam F; Ragab, Marwa A A; Kamal, Miranda F

2017-01-01

Two new, simple, and specific green analytical methods are proposed: zero-crossing first-derivative and chemometric-based spectrophotometric artificial neural network (ANN). The proposed methods were used for the simultaneous estimation of two closely related antioxidant nutraceuticals, coenzyme Q10 (Q10) and vitamin E, in their mixtures and pharmaceutical preparations. The first method is based on the handling of spectrophotometric data with the first-derivative technique, in which both nutraceuticals were determined in ethanol, each at the zero crossing of the other. The amplitudes of the first-derivative spectra for Q10 and vitamin E were recorded at 285 and 235 nm respectively, and correlated with their concentrations. The linearity ranges of Q10 and vitamin E were 10-60 and 5.6-70 μg⋅mL-1, respectively. The second method, ANN, is a multivariate calibration method and it was developed and applied for the simultaneous determination of both analytes. A training set of 90 different synthetic mixtures containing Q10 and vitamin E in the ranges of 0-100 and 0-556 μg⋅mL-1, respectively, was prepared in ethanol. The absorption spectra of the training set were recorded in the spectral region of 230-300 nm. By relating the concentration sets (x-block) with their corresponding absorption data (y-block), gradient-descent back-propagation ANN calibration could be computed. To validate the proposed network, a set of 45 synthetic mixtures of the two drugs was used. Both proposed methods were successfully applied for the assay of Q10 and vitamin E in their laboratory-prepared mixtures and in their pharmaceutical tablets with excellent recovery. These methods offer advantages over other methods because of low-cost equipment, time-saving measures, and environmentally friendly materials. In addition, no chemical separation prior to analysis was needed. The ANN method was superior to the derivative technique because ANN can determine both drugs under nonlinear experimental

Spectrophotometric Determination of Iron(II) and Cobalt(II) by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone

PubMed Central

Devi, V. S. Anusuya; Reddy, V. Krishna

2012-01-01

Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH) reacts with iron(II) and cobalt(II) to form reddish-brown and yellow-coloured [Fe(II)-HNAHBH] and [Co(II)-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II)-HNAHBH], Beer's law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II)-HNAHBH] complex obeys Beer's law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content. PMID:22505925

Application of different spectrophotometric methods for simultaneous determination of elbasvir and grazoprevir in pharmaceutical preparation

NASA Astrophysics Data System (ADS)

Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Abdelazim, Ahmed H.

2018-01-01

The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form. These methods include simultaneous equation, partial least squares with and without variable selection procedure (genetic algorithm). For simultaneous equation method, the absorbance values at 369 (λmax of elbasvir) and 253 nm (λmax of grazoprevir) have been selected for the formation of two simultaneous equations required for the mathematical processing and quantitative analysis of the studied drugs. Alternatively, the partial least squares with and without variable selection procedure (genetic algorithm) have been applied in the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than by using a single or dual wavelength which greatly increases the precision and predictive ability of the methods. Successfully assay of the drugs in their pharmaceutical formulation has been done by the proposed methods. Statistically comparative analysis for the obtained results with the manufacturing methods has been performed. It is noteworthy to mention that there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.

Four Derivative Spectrophotometric Methods for the Simultaneous Determination of Carmoisine and Ponceau 4R in Drinks and Comparison with High Performance Liquid Chromatography

PubMed Central

Turak, Fatma; Dinç, Mithat; Dülger, Öznur; Özgür, Mahmure Ustun

2014-01-01

Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130). PMID:24672549

A comparative study of progressive versus successive spectrophotometric resolution techniques applied for pharmaceutical ternary mixtures.

PubMed

Saleh, Sarah S; Lotfy, Hayam M; Hassan, Nagiba Y; Salem, Hesham

2014-11-11

This work represents a comparative study of a novel progressive spectrophotometric resolution technique namely, amplitude center method (ACM), versus the well-established successive spectrophotometric resolution techniques namely; successive derivative subtraction (SDS); successive derivative of ratio spectra (SDR) and mean centering of ratio spectra (MCR). All the proposed spectrophotometric techniques consist of several consecutive steps utilizing ratio and/or derivative spectra. The novel amplitude center method (ACM) can be used for the determination of ternary mixtures using single divisor where the concentrations of the components are determined through progressive manipulation performed on the same ratio spectrum. Those methods were applied for the analysis of the ternary mixture of chloramphenicol (CHL), dexamethasone sodium phosphate (DXM) and tetryzoline hydrochloride (TZH) in eye drops in the presence of benzalkonium chloride as a preservative. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs. The proposed methods were validated according to the ICH guidelines. A comparative study was conducted between those methods regarding simplicity, limitation and sensitivity. The obtained results were statistically compared with those obtained from the official BP methods, showing no significant difference with respect to accuracy and precision. Copyright © 2014 Elsevier B.V. All rights reserved.

Different spectrophotometric methods applied for the analysis of simeprevir in the presence of its oxidative degradation product: Acomparative study

NASA Astrophysics Data System (ADS)

Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Serag, Ahmed

2018-02-01

Five simple spectrophotometric methods were developed for the determination of simeprevir in the presence of its oxidative degradation product namely, ratio difference, mean centering, derivative ratio using the Savitsky-Golay filters, second derivative and continuous wavelet transform. These methods are linear in the range of 2.5-40 μg/mL and validated according to the ICH guidelines. The obtained results of accuracy, repeatability and precision were found to be within the acceptable limits. The specificity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. Furthermore, these methods were statistically comparable to RP-HPLC method and good results were obtained. So, they can be used for the routine analysis of simeprevir in quality-control laboratories.

Spectrophotometric determination of dopaminergic drugs used for Parkinson's disease, cabergoline and ropinirole, in pharmaceutical preparations.

PubMed

Onal, Armağan; Cağlar, Sena

2007-04-01

Simple and reproducible spectrophotometric methods have been developed for determination of dopaminergic drugs used for Parkinson's disease, cabergoline (CAB) and ropinirole hydrochloride (ROP), in pharmaceutical preparations. The methods are based on the reactions between the studied drug substances and ion-pair agents [methyl orange (MO), bromocresol green (BCG) and bromophenol blue (BPB)] producing yellow colored ion-pair complexes in acidic buffers, after extracting in dichloromethane, which are spectrophotometrically determined at the appropriate wavelength of ion-pair complexes. Beer's law was obeyed within the concentration range from 1.0 to 35 microg ml(-1). The developed methods were applied successfully for the determination of these drugs in tablets.

Fully automated analytical procedure for propofol determination by sequential injection technique with spectrophotometric and fluorimetric detections.

PubMed

Šrámková, Ivana; Amorim, Célia G; Sklenářová, Hana; Montenegro, Maria C B M; Horstkotte, Burkhard; Araújo, Alberto N; Solich, Petr

2014-01-01

In this work, an application of an enzymatic reaction for the determination of the highly hydrophobic drug propofol in emulsion dosage form is presented. Emulsions represent a complex and therefore challenging matrix for analysis. Ethanol was used for breakage of a lipid emulsion, which enabled optical detection. A fully automated method based on Sequential Injection Analysis was developed, allowing propofol determination without the requirement of tedious sample pre-treatment. The method was based on spectrophotometric detection after the enzymatic oxidation catalysed by horseradish peroxidase and subsequent coupling with 4-aminoantipyrine leading to a coloured product with an absorbance maximum at 485 nm. This procedure was compared with a simple fluorimetric method, which was based on the direct selective fluorescence emission of propofol in ethanol at 347 nm. Both methods provide comparable validation parameters with linear working ranges of 0.005-0.100 mg mL(-1) and 0.004-0.243 mg mL(-1) for the spectrophotometric and fluorimetric methods, respectively. The detection and quantitation limits achieved with the spectrophotometric method were 0.0016 and 0.0053 mg mL(-1), respectively. The fluorimetric method provided the detection limit of 0.0013 mg mL(-1) and limit of quantitation of 0.0043 mg mL(-1). The RSD did not exceed 5% and 2% (n=10), correspondingly. A sample throughput of approx. 14 h(-1) for the spectrophotometric and 68 h(-1) for the fluorimetric detection was achieved. Both methods proved to be suitable for the determination of propofol in pharmaceutical formulation with average recovery values of 98.1 and 98.5%. © 2013 Elsevier B.V. All rights reserved.

Rapid and on-site analysis of illegal drugs on the nano-microscale using a deep ultraviolet-visible reflected optical fiber sensor.

PubMed

Li, Qiang; Qiu, Tian; Hao, Hongxia; Zhou, Hong; Wang, Tongzhou; Zhang, Ye; Li, Xin; Huang, Guoliang; Cheng, Jing

2012-04-07

A deep ultraviolet-visible (DUV-Vis) reflected optical fiber sensor was developed for use in a simple spectrophotometric detection system to detect the absorption of various illegal drugs at wavelengths between 180 and 800 nm. Quantitative analyses performed using the sensor revealed a high specificity and sensitivity for drug detection at a wavelength of approximately 200 nm. Using a double-absorption optical path length, extremely small sample volumes were used (32 to 160 nL), which allowed the use of minimal amounts of samples. A portable spectrophotometric system was established based on our optical fiber sensor for the on-site determination and quantitative analysis of common illegal drugs, such as 3,4-methylenedioxymethamphetamine (MDMA), ketamine hydrochloride, cocaine hydrochloride, diazepam, phenobarbital, and barbital. By analyzing the absorbance spectra, six different drugs were quantified at concentrations that ranged from 0.1 to 1000 μg mL(-1) (16 pg-0.16 μg). A novel Matching Algorithm of Spectra Space (MASS) was used to accurately distinguish between each drug in a mixture. As an important supplement to traditional methods, such as mass spectrometry or chromatography, our optical fiber sensor offers rapid and low-cost on-site detection using trace amounts of sample. This rapid and accurate analytical method has wide-ranging applications in forensic science, law enforcement, and medicine.

Miniaturized and direct spectrophotometric multi-sample analysis of trace metals in natural waters.

PubMed

Albendín, Gemma; López-López, José A; Pinto, Juan J

2016-03-15

Trends in the analysis of trace metals in natural waters are mainly based on the development of sample treatment methods to isolate and pre-concentrate the metal from the matrix in a simpler extract for further instrumental analysis. However, direct analysis is often possible using more accessible techniques such as spectrophotometry. In this case a proper ligand is required to form a complex that absorbs radiation in the ultraviolet-visible (UV-Vis) spectrum. In this sense, the hydrazone derivative, di-2-pyridylketone benzoylhydrazone (dPKBH), forms complexes with copper (Cu) and vanadium (V) that absorb light at 370 and 395 nm, respectively. Although spectrophotometric methods are considered as time- and reagent-consuming, this work focused on its miniaturization by reducing the volume of sample as well as time and cost of analysis. In both methods, a micro-amount of sample is placed into a microplate reader with a capacity for 96 samples, which can be analyzed in times ranging from 5 to 10 min. The proposed methods have been optimized using a Box-Behnken design of experiments. For Cu determination, concentration of phosphate buffer solution at pH 8.33, masking agents (ammonium fluoride and sodium citrate), and dPKBH were optimized. For V analysis, sample (pH 4.5) was obtained using acetic acid/sodium acetate buffer, and masking agents were ammonium fluoride and 1,2-cyclohexanediaminetetraacetic acid. Under optimal conditions, both methods were applied to the analysis of certified reference materials TMDA-62 (lake water), LGC-6016 (estuarine water), and LGC-6019 (river water). In all cases, results proved the accuracy of the method. Copyright © 2015 Elsevier Inc. All rights reserved.

Ultraviolet and visible light spectrophotometric approach to blood typing: objective analysis by agglutination index.

PubMed

Narayanan, S; Orton, S; Leparc, G F; Garcia-Rubio, L H; Potter, R L

1999-10-01

A new blood typing technology based on ultraviolet (UV) and visible light spectroscopy (UV/visible spectroscopy) has been developed. Blood groups and types are determined by quantifying reproducible changes in the UV and visible light spectra of blood in the presence of agglutinating antibodies. Samples of red cells in the presence and absence of agglutinating antibodies were examined by UV/visible spectroscopy. Blood groups and types were determined by comparing the optical density spectra obtained between 665 and 1000 nm. These comparisons generate numbers (agglutination index) ranging from 0 to 100, with smaller numbers corresponding to lack of agglutination and larger numbers corresponding to agglutination. The optical density of agglutinated blood is dramatically different from that of unagglutinated blood. The agglutination index derived from the relative slopes of the spectra is an objective indicator of agglutination strength. An agglutination index greater than 17 consistently and accurately established blood group- and type-specific agglutination. The method accurately predicted A, B, and O blood groups, and D type in over 275 samples. Scattering theory-based calculations of relative volumes of red cells before and after agglutination show a direct correlation with the agglutination index and provide the theoretical basis of the analysis. This quantitative technique is reproducible and has the potential for automation.

Polymerization Evaluation by Spectrophotometric Measurements.

ERIC Educational Resources Information Center

Dunach, Jaume

1985-01-01

Discusses polymerization evaluation by spectrophotometric measurements by considering: (1) association degrees and molar absorptivities; (2) association degrees and equilibrium constants; and (3) absorbance and equilibrium constants. (JN)

A Spectrophotometric Study of the Permanganate-Oxalate Reaction: An Analytical Laboratory Experiment

ERIC Educational Resources Information Center

Kalbus, Gene E.; Lieu, Van T.; Kalbus, Lee H.

2004-01-01

The spectrophotometric method assists in the study of potassium permanganate-oxalate reaction. Basic analytical techniques and rules are implemented in the experiment, which can also include the examination of other compounds oxidized by permanganate.

Catalytic spectrophotometric determination of iodide in pharmaceutical preparations and edible salt.

PubMed

El-Ries, M A; Khaled, Elmorsy; Zidane, F I; Ibrahim, S A; Abd-Elmonem, M S

2012-02-01

The catalytic effect of iodide on the oxidation of four dyes: viz. variamine blue (VB), methylene blue (MB), rhodamine B (RB), and malachite green (MG) with different oxidizing agents was investigated for the kinetic spectrophotometric determination of iodide. The above catalyzed reactions were monitored spectrophotometrically by following the change in dye absorbances at 544, 558, 660, or 617 nm for the VB, RB, MB, or MG catalyzed reactions, respectively. Under optimum conditions, iodide can be determined within the concentration levels 0.064-1.27 µg mL(-1) for VB method, 3.20-9.54 µg mL(-1) for RB method, 5.00-19.00 µg mL(-1) for the MB method, and 6.4-19.0 µg mL(-1) for the MG one, with detection limit reaching 0.004 µg mL(-1) iodide. The reported methods were highly sensitive, selective, and free from most interference. Applying the proposed procedures, trace amounts of iodide in pharmaceutical and edible salt samples were successfully determined without separation or pretreatment steps. Copyright © 2011 John Wiley & Sons, Ltd.

Spectrophotometric techniques to determine tranexamic acid: Kinetic studies using ninhydrin and direct measuring using ferric chloride

NASA Astrophysics Data System (ADS)

Arayne, M. Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed; Mirza, Agha Zeeshan; Zuberi, M. Hashim

2008-11-01

Two simple and sensitive spectrophotometric methods in ultraviolet and visible region are described for the determination of tranexamic acid in pure form and pharmaceutical preparations. The first method is based on the reaction of the drug with ninhydrin at boiling temperature and by measuring the increase in absorbance at 575 nm as a function of time. The initial rate, rate constant and fixed time (120 min) procedures were used for constructing the calibration graphs to determine the concentration of the drug, which showed a linear response over the concentration range 16-37 μg mL -1 with correlation coefficient " r" 0.9997, 0.996, 0.9999, LOQ 6.968, 7.138, 2.462 μgmL -1 and LOD 2.090, 2.141 and 0.739 μgmL -1, respectively. In second method tranexamic acid was reacted with ferric chloride solution, yellowish orange colored chromogen showed λ max at 375 nm showing linearity in the concentration range of 50-800 μg mL -1 with correlation coefficient " r" 0.9997, LOQ 6.227 μgmL -1 and LOD 1.868 μgmL -1. The variables affecting the development of the color were optimized and the developed methods were validated statistically and through recovery studies. These results were also verified by IR and NMR spectroscopy. The proposed methods have been successfully applied to the determination of tranexamic acid in commercial pharmaceutical formulation.

Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

PubMed

Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

2016-05-01

Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

Spectrophotometric determination of the total flavonoid content in Ocimum basilicum L. (Lamiaceae) leaves

PubMed Central

da Silva, Layzon Antonio Lemos; Pezzini, Bianca Ramos; Soares, Luciano

2015-01-01

Background: The chemical characterization is essential to validate the pharmaceutical use of vegetable raw materials. Ultraviolet spectroscopy is an important technique to determine flavonoids, which are important active compounds from Ocimum basilicum. Objective: The objective of this work was to optimize a spectrophotometric method, based on flavonoid-aluminum chloride (AlCl3) complexation to determine the total flavonoid content (TFC) in leaves of O. basilicum (herbal material), using response surface methodology. Materials and Methods: The effects of (1) the herbal material: Solvent ratio (0.02, 0.03, 0.05, 0.07, and 0.08 g/mL), (2) stock solution volume (0.8, 2.3, 4.4, 6.5, and 8.0 mL) and (3) AlCl3 volume (0.8, 1.0, 1.2, 1.4, and 1.6 mL) on the TFC were evaluated. The analytical performance parameters precision, linearity and robustness of the method were tested. Results: The herbal material: Solvent ratio and stock solution volume showed an important influence on the method response. After choosing the optimized conditions, the method exhibited a precision (RSD%) lower than 6% for repeatability (RSD%) and lower than 8% for intermediate precision (on the order of literature values for biotechnological methods), coefficient of correlation of 0.9984, and no important influence could be observed for variations of the time of complexation with AlCl3. However, the time and temperature of extraction were critical for TFC method and must be carefully controlled during the analysis. Conclusion: Thus, this study allowed the optimization of a simple, fast and precise method for the determination of the TFC in leaves of O. basilicum, which can be used to support the quality assessment of this herbal material. PMID:25709217

Comparative Validation of the Determination of Sofosbuvir in Pharmaceuticals by Several Inexpensive Ecofriendly Chromatographic, Electrophoretic, and Spectrophotometric Methods.

PubMed

El-Yazbi, Amira F

2017-07-01

Sofosbuvir (SOFO) was approved by the U.S. Food and Drug Administration in 2013 for the treatment of hepatitis C virus infection with enhanced antiviral potency compared with earlier analogs. Notwithstanding, all current editions of the pharmacopeias still do not present any analytical methods for the quantification of SOFO. Thus, rapid, simple, and ecofriendly methods for the routine analysis of commercial formulations of SOFO are desirable. In this study, five accurate methods for the determination of SOFO in pharmaceutical tablets were developed and validated. These methods include HPLC, capillary zone electrophoresis, HPTLC, and UV spectrophotometric and derivative spectrometry methods. The proposed methods proved to be rapid, simple, sensitive, selective, and accurate analytical procedures that were suitable for the reliable determination of SOFO in pharmaceutical tablets. An analysis of variance test with P-value > 0.05 confirmed that there were no significant differences between the proposed assays. Thus, any of these methods can be used for the routine analysis of SOFO in commercial tablets.

Simultaneous spectrophotometric determination of paracetamol and salicylamide in human serum and pharmaceutical formulations by a differential kinetic method.

PubMed

Zarei, Ali Reza; Afkhami, Abbas; Sarlak, Nahid

2005-01-01

A rapid, simple, and sensitive differential kinetic method is presented for the determinations of acetaminophen (also known as paracetamol) and salicylamide. The method is based on their oxidation reaction by Fe3+ ion in the presence of 1, 10-phenanthroline as indicator. The reactions can be monitored spectrophotometrically by measuring the increase in the absorbance of the solution at 510 nm. Two times were selected one in which only paracetamol is oxidized by Fe3+ ion and the other in which both drugs are oxidized by Fe3+ ion. The data were evaluated by the proportional equations method. The method allowed the simultaneous determination of paracetamol and salicylamide at concentrations between 0.5-20 and 1-40 microg/mL with relative standard deviations of 3.47 and 2.58%, respectively. The method was applied to the simultaneous determination of paracetamol and salicylamide in human serum and pharmaceutical formulations.

Antioxidant activity profiling by spectrophotometric methods of aqueous methanolic extracts of Helichrysum stoechas subsp. rupestre and Phagnalon saxatile subsp. saxatile.

PubMed

Haddouchi, Farah; Chaouche, Tarik Mohammed; Ksouri, Riadh; Medini, Faten; Sekkal, Fatima Zohra; Benmansour, Abdelhafid

2014-06-01

The aqueous methanolic extracts of two plants from Algeria, Helichrysum stoechas subsp. rupestre and Phagnalon saxatile subsp. saxatile, were investigated for their antioxidant activity. Total phenolics, flavonoids, and tannins were determined by spectrophotometric techniques. In vitro antioxidant and radical scavenging profiling was determined by spectrophotometric methods, through: Total antioxidant capacity, and radical scavenging effects by the DPPH and ABTS methods, reducing and chelating power, and blanching inhibition of the β-carotene. All of the extracts showed interesting antioxidant and radical scavenging activity. The highest contents in phenolics, tannins, and the highest total antioxidant capacity as gallic acid equivalents of 97.5 ± 0.33 mg GAE/g DW was obtained for the flowers of H. stoechas subsp. rupestre extract in the phosphomolybdenum assay. An extract of the leafy stems of P. saxatile subsp. saxatile revealed the highest content of flavonoids, and the highest antioxidant activity by the radical scavenging and β-carotene assays when compared with standards. The best activity was by the scavenging radical DPPH with an IC50 value of 5.65 ± 0.10 μg·mL(-1). The studied medicinal plants could provide scientific evidence for some traditional uses in the treatment of diseases related to the production of reactive oxygen species (ROS) and oxidative stress. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Two different spectrophotometric determinations of potential anticancer drug and its toxic metabolite

NASA Astrophysics Data System (ADS)

Farid, Nehal F.; Abdelwahab, Nada S.

2015-06-01

Flutamide is a hormone therapy used for men with advanced prostate cancer. Flutamide is highly susceptible to hydrolysis with the production of 3-(trifluoromethyl)aniline, which is reported to be one of its toxic metabolites, impurities and related substances according to BP and USP. Flutamide was found to be stable when exposed to oxidation by 30% hydrogen peroxide and direct sunlight for up to 4 h. Two accurate and sensitive spectrophotometric methods were used for determination of flutamide in bulk and in pharmaceutical formulations. Method (I) is the area under curve (AUC) spectrophotometric method that depends on measuring the AUC in the wavelength ranges of 275-305 nm and 350-380 nm and using Cramer's rule. The linearity range was found to be 1-35 μg/mL and 0.5-16 μg/mL for the drug and the degradate, respectively. In method (II), combination of the isoabsorptive and dual wavelength spectrophotometric methods was used for resolving the binary mixture. The absorbance at 249.2 nm (λiso) was used for determination of total mixture concentration, while the difference in absorbance between 232 nm and 341.2 nm was used for measuring the drug concentration. By subtraction, the degradate concentration was obtained. Beer's law was obeyed in the range of 2-35 μg/mL and 0.5-20 μg/mL for the drug and its degradate, respectively. The two methods were validated according to USP guidelines and were applied for determination of the drug in its pharmaceutical dosage form. Moreover AUC method was used for the kinetic study of the hydrolytic degradation of flutamide. The kinetic degradation of flutamide was found to follow pseudo-first order kinetics and is pH and temperature dependent. Activation energy, kinetic rate constants and t1/2 at different temperatures and pH values were calculated.

Hypothesis testing for the validation of the kinetic spectrophotometric methods for the determination of lansoprazole in bulk and drug formulations via Fe(III) and Zn(II) chelates.

PubMed

Rahman, Nafisur; Kashif, Mohammad

2010-03-01

Point and interval hypothesis tests performed to validate two simple and economical, kinetic spectrophotometric methods for the assay of lansoprazole are described. The methods are based on the formation of chelate complex of the drug with Fe(III) and Zn(II). The reaction is followed spectrophotometrically by measuring the rate of change of absorbance of coloured chelates of the drug with Fe(III) and Zn(II) at 445 and 510 nm, respectively. The stoichiometric ratio of lansoprazole to Fe(III) and Zn(II) complexes were found to be 1:1 and 2:1, respectively. The initial-rate and fixed-time methods are adopted for determination of drug concentrations. The calibration graphs are linear in the range 50-200 µg ml⁻¹ (initial-rate method), 20-180 µg ml⁻¹ (fixed-time method) for lansoprazole-Fe(III) complex and 120-300 (initial-rate method), and 90-210 µg ml⁻¹ (fixed-time method) for lansoprazole-Zn(II) complex. The inter-day and intra-day precision data showed good accuracy and precision of the proposed procedure for analysis of lansoprazole. The point and interval hypothesis tests indicate that the proposed procedures are not biased. Copyright © 2010 John Wiley & Sons, Ltd.

Novel kinetic spectrophotometric method for estimation of certain biologically active phenolic sympathomimetic drugs in their bulk powders and different pharmaceutical formulations

NASA Astrophysics Data System (ADS)

Omar, Mahmoud A.; Badr El-Din, Khalid M.; Salem, Hesham; Abdelmageed, Osama H.

2018-03-01

A simple, selective and sensitive kinetic spectrophotometric method was described for estimation of four phenolic sympathomimetic drugs namely; terbutaline sulfate, fenoterol hydrobromide, isoxsuprine hydrochloride and etilefrine hydrochloride. This method is depended on the oxidation of the phenolic drugs with Folin-Ciocalteu reagent in presence of sodium carbonate. The rate of color development at 747-760 nm was measured spectrophotometrically. The experimental parameters controlling the color development were fully studied and optimized. The reaction mechanism for color development was proposed. The calibration graphs for both the initial rate and fixed time methods were constructed, where linear correlations were found in the general concentration ranges of 3.65 × 10- 6-2.19 × 10- 5 mol L- 1 and 2-24.0 μg mL- 1 with correlation coefficients in the following range 0.9992-0.9999, 0.9991-0.9998 respectively. The limits of detection and quantitation for the initial rate and fixed time methods were found to be in general concentration range 0.109-0.273, 0.363-0.910 and 0.210-0.483, 0.700-1.611 μg mL- 1 respectively. The developed method was validated according to ICH and USP 30 -NF 25 guidelines. The suggested method was successfully implemented to the estimation of these drugs in their commercial pharmaceutical formulations and the recovery percentages obtained were ranged from 97.63% ± 1.37 to 100.17% ± 0.95 and 97.29% ± 0.74 to 100.14 ± 0.81 for initial rate and fixed time methods respectively. The data obtained from the analysis of dosage forms were compared with those obtained by reported methods. Statistical analysis of these results indicated no significant variation in the accuracy and precision of both the proposed and reported methods.

Comparison of Spectrophotometric Methods for the Determination of Copper in Sugar Cane Spirit.

PubMed

Soares, Sarah Adriana R; Costa, Silvânio Silvério L; Araujo, Rennan Geovanny O; Teixeira, Leonardo Sena Gomes; Dantas, Alailson Falcão

2018-05-01

Three spectrophotometric methods were developed for the determination of copper (Cu) in sugar cane spirit using the chromogenic reagents neocuproine, cuprizone, and bathocuproine. Experimental conditions, such as reagent concentration, reducer concentration, pH, buffer concentration, the order of addition of reagents, and the stability of the complexes, were optimized. The work range was established from 1.0 to 10.0 µg/mL, with correlation coefficients of >0.999 for all three optimized methods. The methods were evaluated regarding accuracy by addition and recovery tests at five concentration levels, and the obtained recoveries ranged from 91 to 105% (n = 3). Precision was expressed as RSD (relative standard deviation), with values ranging from 0.01 to 0.17% (n = 10). The method using the chromogenic reagent cuprizone presented the greatest molar absorptivity, followed by bathocuproine and neocuproine. The methods were applied for the determination of Cu in sugar cane spirit, and the results were compared with a reference method by flame atomic absorption spectrometry (FAAS). Calibration curve solutions for FAAS analysis were prepared in a 40% (v/v) alcohol medium in a range of concentrations from 0.5 up to 5 µg/mL. Measurements for Cu determination were carried out at a wavelength of 324.7 nm. The concentrations obtained for Cu in sugar cane spirit samples from Brazil were between 1.99 and 12.63 µg/mL, and about 75% of the samples presented Cu concentrations above the limit established by Brazilian legislation (5.0 µg/mL or 5.0 mg/L).

Spectrofluorimetric and spectrophotometric stability-indicating methods for determination of some oxicams using 7-chloro-4-nitrobenz-2-oxa-1,3-diazole (NBD-Cl).

PubMed

Taha, Elham Anwer; Salama, Nahla Nour; Fattah, Laila El-Sayed Abdel

2006-05-01

Two sensitive and selective spectrofluorimetric and spectrophotometric stability-indicating methods have been developed for the determination of some non-steroidal anti-inflammatory oxicam derivatives namely lornoxicam (Lx), tenoxicam (Tx) and meloxicam (Mx) after their complete alkaline hydrolysis. The methods are based on derivatization of alkaline hydrolytic products with 7-chloro-4-nitrobenz-2-oxa-1,3-diazole (NBD-Cl). The products showed an absorption maximum at 460 nm for the three studied drugs and fluorescence emission peak at 535 nm in methanol. The color was stable for at least 48 h. The optimum conditions of the reaction were investigated and it was found that the reaction proceeds quantitatively at pH 8, after heating in a boiling water bath for 30 min. The methods were found to be linear in the ranges of 1-10 microg ml(-1) for Lx and Tx and 0.5-4.0 microg ml(-1) for Mx for spectrophotometric method, while 0.05-1.0 microg ml(-1) for Lx and Tx and 0.025-0.4 microg ml(-1) for Mx for the spectrofluorimetric method. The validity of the methods was assessed according to USP guidelines. Statistical analysis of the results revealed high accuracy and good precision. The suggested procedures could be used for the determination of the above mentioned drugs in pure and dosage forms as well as in the presence of their degradation products.

Spectrophotometric determination of triclosan based on diazotization reaction: response surface optimization using Box-Behnken design.

PubMed

Kaur, Inderpreet; Gaba, Sonal; Kaur, Sukhraj; Kumar, Rajeev; Chawla, Jyoti

2018-05-01

A spectrophotometric method based on diazotization of aniline with triclosan has been developed for the determination of triclosan in water samples. The diazotization process involves two steps: (1) reaction of aniline with sodium nitrite in an acidic medium to form diazonium ion and (2) reaction of diazonium ion with triclosan to form a yellowish-orange azo compound in an alkaline medium. The resulting yellowish-orange product has a maximum absorption at 352 nm which allows the determination of triclosan in aqueous solution in the linear concentration range of 0.1-3.0 μM with R 2 = 0.998. The concentration of hydrochloric acid, sodium nitrite, and aniline was optimized for diazotization reaction to achieve good spectrophotometric determination of triclosan. The optimization of experimental conditions for spectrophotometric determination of triclosan in terms of concentration of sodium nitrite, hydrogen chloride and aniline was also carried out by using Box-Behnken design of response surface methodology and results obtained were in agreement with the experimentally optimized values. The proposed method was then successfully applied for analyses of triclosan content in water samples.

SPECTROPHOTOMETRIC DETERMINATION OF TRACES OF BORON IN THORIUM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Onishi, H.; Ishiwatari, N.; Nagai, H.

1960-12-01

A procedure is described for the spectrophotometric determination of a few tenths of a pant per million of boron ia thorium oxide or thorium. The sample is dissolved in strong phosphoric acid. After diluting the solution with water, boron is separated by distillation as methyl borate and finally determined by the curcumin method. The error is not likely to exceed plus or minus O.l ppm for 0.2 to 1 ppm of boron. (auth)

Proceedings of the Workshop on the Spectrophotometric Dating of Stars and Galaxies

NASA Technical Reports Server (NTRS)

Hubeny, Ivan; Heap, Sara; Cornett, Robert

1999-01-01

In the past decade, we have seen an avalanche of new observational results from space observatories and ground-based observatories. These observations have revealed young globular clusters in the cores of merger galaxies, elliptical galaxies at redshifts up to z=1.5, and starburst galaxies at high redshift. Analyses of the detailed spectra or color- magnitude diagrams of these systems promise to give a new understanding of evolutionary processes and to provide a check on cosmological ages. At the same time, these new spectro-photometric data present new challenges to current methods of spectral analysis and modeling.At the Workshop, we will discuss these new opportunities and challenges on spectro-photometric dating of stars and galaxies.

Simultaneous spectrophotometric determination of crystal violet and malachite green in water samples using partial least squares regression and central composite design after preconcentration by dispersive solid-phase extraction.

PubMed

Razi-Asrami, Mahboobeh; Ghasemi, Jahan B; Amiri, Nayereh; Sadeghi, Seyed Jamal

2017-04-01

In this paper, a simple, fast, and inexpensive method is introduced for the simultaneous spectrophotometric determination of crystal violet (CV) and malachite green (MG) contents in aquatic samples using partial least squares regression (PLS) as a multivariate calibration technique after preconcentration by graphene oxide (GO). The method was based on the sorption and desorption of analytes onto GO and direct determination by ultraviolet-visible spectrophotometric techniques. GO was synthesized according to Hummers method. To characterize the shape and structure of GO, FT-IR, SEM, and XRD were used. The effective factors on the extraction efficiency such as pH, extraction time, and the amount of adsorbent were optimized using central composite design. The optimum values of these factors were 6, 15 min, and 12 mg, respectively. The maximum capacity of GO for the adsorption of CV and MG was 63.17 and 77.02 mg g -1 , respectively. Preconcentration factors and extraction recoveries were obtained and were 19.6, 98% for CV and 20, 100% for MG, respectively. LOD and linear dynamic ranges for CV and MG were 0.009, 0.03-0.3, 0.015, and 0.05-0.5 (μg mL -1 ), respectively. The intra-day and inter-day relative standard deviations were 1.99 and 0.58 for CV and 1.69 and 3.13 for MG at the concentration level of 50 ng mL -1 , respectively. Finally, the proposed DSPE/PLS method was successfully applied for the simultaneous determination of the trace amount of CV and MG in the real water samples.

New simple spectrophotometric method for determination of the binary mixtures (atorvastatin calcium and ezetimibe; candesartan cilexetil and hydrochlorothiazide) in tablets.

PubMed

Belal, Tarek S; Daabees, Hoda G; Abdel-Khalek, Magdi M; Mahrous, Mohamed S; Khamis, Mona M

2013-04-01

A new simple spectrophotometric method was developed for the determination of binary mixtures without prior separation. The method is based on the generation of ratio spectra of compound X by using a standard spectrum of compound Y as a divisor. The peak to trough amplitudes between two selected wavelengths in the ratio spectra are proportional to concentration of X without interference from Y . The method was demonstrated by determination of two drug combinations. The first consists of the two antihyperlipidemics: atorvastatin calcium (ATV) and ezetimibe (EZE), and the second comprises the antihypertensives: candesartan cilexetil (CAN) and hydrochlorothiazide (HCT). For mixture 1, ATV was determined using 10 μg/mL EZE as the divisor to generate the ratio spectra, and the peak to trough amplitudes between 231 and 276 nm were plotted against ATV concentration. Similarly, by using 10 μg/mL ATV as divisor, the peak to trough amplitudes between 231 and 276 nm were found proportional to EZE concentration. Calibration curves were linear in the range 2.5-40 μg/mL for both drugs. For mixture 2, divisor concentration was 7.5 μg/mL for both drugs. CAN was determined using its peak to trough amplitudes at 251 and 277 nm, while HCT was estimated using the amplitudes between 251 and 276 nm. The measured amplitudes were linearly correlated to concentration in the ranges 2.5-50 and 1-30 μg/mL for CAN and HCT, respectively. The proposed spectrophotometric method was validated and successfully applied for the assay of both drug combinations in several laboratory-prepared mixtures and commercial tablets.

Simple Ultraviolet Short-Pulse Intensity Diagnostic Method Using Atmosphere

NASA Astrophysics Data System (ADS)

Aota, Tatsuya; Takahashi, Eiichi; Losev, Leonid L.; Tabuchi, Takeyuki; Kato, Susumu; Matsumoto, Yuji; Okuda, Isao; Owadano, Yoshiro

2005-05-01

An ultraviolet (UV) short-pulse intensity diagnostic method using atmosphere as a nonlinear medium was developed. This diagnostic method is based on evaluating the ion charge of the two-photon ionization of atmospheric oxygen upon irradiation with a UV (238-299 nm) short-pulse laser. The observed ion signal increased proportionally to the input intensity to the power of ˜2.2, during the two-photon ionization of atmospheric oxygen. An autocorrelator was constructed and used to successfully measure a UV laser pulse of ˜400 fs duration. Since this diagnostic system is used in the open-air under windowless conditions, it can be set along the beam path and used as a UV intensity monitor.

A Microscale Spectrophotometric Determination of Water Hardness

NASA Astrophysics Data System (ADS)

Gordon, James S.

2001-08-01

A spectrophotometric titration was performed to determine water hardness. The titration incorporated the traditional titration method employing EDTA as the titrant and calmagite as the indicator. The microscale experiment was carried out in a spectrometer cuvette and made use of a Texas Instruments (TI-83) calculator interfaced through a TI Calculator-Based Laboratory system to a Vernier colorimeter as the detector. Monitoring at 635 nm, one of the colorimeter's fixed wavelengths, was well suited for this analysis. Agreement was found with results from traditional titrations.

A NOISE ADAPTIVE FUZZY EQUALIZATION METHOD FOR PROCESSING SOLAR EXTREME ULTRAVIOLET IMAGES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Druckmueller, M., E-mail: druckmuller@fme.vutbr.cz

A new image enhancement tool ideally suited for the visualization of fine structures in extreme ultraviolet images of the corona is presented in this paper. The Noise Adaptive Fuzzy Equalization method is particularly suited for the exceptionally high dynamic range images from the Atmospheric Imaging Assembly instrument on the Solar Dynamics Observatory. This method produces artifact-free images and gives significantly better results than methods based on convolution or Fourier transform which are often used for that purpose.

Validated UV-spectrophotometric method for the evaluation of the efficacy of makeup remover.

PubMed

Charoennit, P; Lourith, N

2012-04-01

A UV-spectrophotometric method for the analysis of makeup remover was developed and validated according to ICH guidelines. Three makeup removers for which the main ingredients consisted of vegetable oil (A), mineral oil and silicone (B) and mineral oil and water (C) were sampled in this study. Ethanol was the optimal solvent because it did not interfere with the maximum absorbance of the liquid foundation at 250 nm. The linearity was determined over a range of makeup concentrations from 0.540 to 1.412 mg mL⁻¹ (R² = 0.9977). The accuracy of this method was determined by analysing low, intermediate and high concentrations of the liquid foundation and gave 78.59-91.57% recoveries with a relative standard deviation of <2% (0.56-1.45%). This result demonstrates the validity and reliability of this method. The reproducibilities were 97.32 ± 1.79, 88.34 ± 2.69 and 95.63 ± 2.94 for preparations A, B and C respectively, which are within the acceptable limits set forth by the ASEAN analytical validation guidelines, which ensure the precision of the method under the same operating conditions over a short time interval and the inter-assay precision within the laboratory. The proposed method is therefore a simple, rapid, accurate, precise and inexpensive technique for the routine analysis of makeup remover efficacy. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Sensitive Indirect Spectrophotometric Method for Determination of H2-Receptor Antagonists in Pharmaceutical Formulations

PubMed Central

Darwish, Ibrahim A.; Hussein, Samiha A.; Mahmoud, Ashraf M.; Hassan, Ahmed I.

2007-01-01

A simple, accurate and sensitive spectrophotometric method has been developed and validated for determination of H2-receptor antagonists: cimetidine, famotidine, nizatidine, and ranitidine hydrochloride. The method was based on the oxidation of these drugs with cerium (IV) in presence of perchloric acid and subsequent measurement of the excess Ce (IV) by its reaction with p-dimethylaminocinnamaldehyde to give a red colored product (λmax at 464 nm). The decrease in the absorption intensity (ΔA) of the colored product, due to the presence of the drug was correlated with its concentration in the sample solution. Different variables affecting the reaction were carefully studied and optimized. Under the optimum conditions, linear relationships with good correlation coefficients (0.9985-0.9994) were found between ΔA values and the concentrations of the drugs in a concentration range of 1-16 µg ml-1. The assay limits of detection and quantitation were 0.12-0.44 and 0.37-1.33 µg ml-1, respectively. The method was validated, in terms of accuracy, precision, ruggedness, and robustness; the results were satisfactory. The proposed method was successfully applied to the analysis of the investigated drugs in their pure and pharmaceutical dosage forms (recovery was 98.8-102.5 ± 0.79-1.72%) without interference from the common excipients. The results obtained by the proposed method were comparable with those obtained by the official methods. PMID:23675034

A novel flow injection spectrophotometric method using plant extracts as green reagent for the determination of doxycycline

NASA Astrophysics Data System (ADS)

Palamy, Sysay; Ruengsitagoon, Wirat

2017-01-01

A novel flow injection spectrophotometric method was developed for the determination of doxycycline in pharmaceutical preparations using iron(III) contained in extracts from plants. The assay was based on the complex formed between doxycycline and iron(III) characterized by an absorption maximum at 435 nm. The calibration graphs obtained over the doxycycline concentration range 5-250 μg mL- 1 gave correlation coefficients of 0.9979, 0.9987 and 0.9987 with the three green reagents prepared from Senna alata (L.) Roxb. (S. alata), Polygonum hydropiper L. (P. hydropiper) or Diplazium esculentum (Retz.) Sw. (D. esculentum), respectively. The relative standard deviations of the repeatability was < 2.00%. The percentage recoveries were in the range of 98.27-101.03%. Doxycycline contents obtained by this new method and by the reference methods reported in literature were in agreement at 95% confidence level with the paired t-test. The sample throughput was 36 h- 1 for each green reagent.

Development of a Rapid Derivative Spectrophotometric Method for Simultaneous Determination of Acetaminophen, Diphenhydramine and Pseudoephedrine in Tablets

PubMed Central

Souri, Effat; Rahimi, Aghil; Shabani Ravari, Nazanin; Barazandeh Tehrani, Maliheh

2015-01-01

A mixture of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride is used for the symptomatic treatment of common cold. In this study, a derivative spectrophotometric method based on zero-crossing technique was proposed for simultaneous determination of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride. Determination of these drugs was performed using the 1D value of acetaminophen at 281.5 nm, 2D value of diphenhydramine hydrochloride at 226.0 nm and 4D value of pseudoephedrine hydrochloride at 218.0 nm. The analysis method was linear over the range of 5-50, 0.25-4, and 0.5-5 µg/mL for acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride, respectively. The within-day and between-day CV and error values for all three compounds were within an acceptable range (CV<2.2% and error<3%). The developed method was used for simultaneous determination of these drugs in pharmaceutical dosage forms and no interference from excipients was observed. PMID:25901150

Development and validation of new spectrophotometric ratio H-point standard addition method and application to gastrointestinal acting drugs mixtures

NASA Astrophysics Data System (ADS)

Yehia, Ali M.

2013-05-01

New, simple, specific, accurate and precise spectrophotometric technique utilizing ratio spectra is developed for simultaneous determination of two different binary mixtures. The developed ratio H-point standard addition method (RHPSAM) was managed successfully to resolve the spectral overlap in itopride hydrochloride (ITO) and pantoprazole sodium (PAN) binary mixture, as well as, mosapride citrate (MOS) and PAN binary mixture. The theoretical background and advantages of the newly proposed method are presented. The calibration curves are linear over the concentration range of 5-60 μg/mL, 5-40 μg/mL and 4-24 μg/mL for ITO, MOS and PAN, respectively. Specificity of the method was investigated and relative standard deviations were less than 1.5. The accuracy, precision and repeatability were also investigated for the proposed method according to ICH guidelines.

Development of a Low Cost, Compact, Spectrophotometric pH Sensor

NASA Astrophysics Data System (ADS)

Spaulding, R. S.; Darlington, R. C.; Beck, J. C.; DeGrandpre, M. D.

2016-02-01

Understanding the ecological impacts of oceanic CO2 uptake in the post-industrial world requires high spatial and temporal resolution measurements of inorganic carbon. Most researchers aim for measuring two of the four inorganic carbon parameters (partial pressure of CO2, total alkalinity, total dissolve inorganic carbon, and pH), in order to fully characterize the carbonate system. While this is desirable in many circumstances, in some cases it may be possible to fully characterize the system using pH and salinity, or even to use pH alone as a proxy to the health of calcifying marine organisms. The development of relatively inexpensive spectrophotometric pH sensors compatible with Lagrangian drifters would greatly improve the ability of researchers to characterize the changing oceanic carbonate system. We have designed and tested a novel, miniaturized, submersible, autonomous opto-fluidic device that can be manufactured at a relatively low cost. The flexible design can be deployed independent of or in tandem with GDP style drifters and will enable spectrophotometric pH technology on a host of drifting platforms and buoys. This device uses a dual wavelength light emitting diode (LED) light source, low volume mixer, and an optical flow-cell mounted to the electronic controller board. Laboratory testing shows that this device measures pH with similar accuracy and precision to other spectrophotometric methods such as the SAMI-pH.

Five different spectrophotometric methods for determination of Amprolium hydrochloride and Ethopabate binary mixture

NASA Astrophysics Data System (ADS)

Hussein, Lobna A.; Magdy, N.; Abbas, Mahmoud M.

2015-03-01

Five simple, specific, accurate and precise UV-spectrophotometric methods are adopted for the simultaneous determination of Amprolium hydrochloride (AMP) and Ethopabate (ETH), a binary mixture with overlapping spectra, without preliminary separation. The first method is first derivative of the ratio spectra (1DD) for determination of AMP and ETH at 234.7 nm and 306.8 nm respectively with mean percentage recoveries 99.76 ± 0.907 and 100.29 ± 0.842 respectively. The second method is the mean centering of the ratio spectra for determination of AMP and ETH at 238.8 nm and 313 nm respectively with mean percentage recoveries 100.26 ± 1.018 and 99.94 ± 1.286 respectively. The third method is based on dual wavelength selection for determination of AMP and ETH at 235.3 nm & 308 nm and 244 nm & 268.4 nm respectively with mean percentage recoveries 99.30 ± 1.097 and 100.03 ± 1.065 respectively. The fourth method is ratio difference method for determination of AMP and ETH at 239 nm & 310 nm and 239 nm & 313 nm respectively with mean percentage recoveries 99.27 ± 0.892 and 100.40 ± 1.814 respectively. The fifth one is area under the curve (AUC) method where the areas between 235.6-243 nm and 268.3-275 nm are selected for determination of AMP and ETH with mean percentage recoveries 100.35 ± 1.031 and 100.39 ± 0.956 respectively. These methods are tested by analyzing synthetic mixtures of the two drugs and they are applied to their pharmaceutical veterinary preparation. Methods are validated according to the ICH guidelines and accuracy, precision and repeatability are found to be within the acceptable limit.

Chromium speciation in environmental samples using a solid phase spectrophotometric method

NASA Astrophysics Data System (ADS)

Amin, Alaa S.; Kassem, Mohammed A.

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

Chromium speciation in environmental samples using a solid phase spectrophotometric method.

PubMed

Amin, Alaa S; Kassem, Mohammed A

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H(2)SO(4) and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11×10(7) and 3.90×10(7) L mol(-1)cm(-1) for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L(-1) with RSD of <1.85% (n=8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L(-1) for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L(-1), respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested. Copyright © 2012 Elsevier B.V. All rights reserved.

A validated fast difference spectrophotometric method for 5-hydroxymethyl-2-furfural (HMF) determination in corn syrups.

PubMed

de Andrade, Jucimara Kulek; de Andrade, Camila Kulek; Komatsu, Emy; Perreault, Hélène; Torres, Yohandra Reyes; da Rosa, Marcos Roberto; Felsner, Maria Lurdes

2017-08-01

Corn syrups, important ingredients used in food and beverage industries, often contain high levels of 5-hydroxymethyl-2-furfural (HMF), a toxic contaminant. In this work, an in house validation of a difference spectrophotometric method for HMF analysis in corn syrups was developed using sophisticated statistical tools by the first time. The methodology showed excellent analytical performance with good selectivity, linearity (R 2 =99.9%, r>0.99), accuracy and low limits (LOD=0.10mgL -1 and LOQ=0.34mgL -1 ). An excellent precision was confirmed by repeatability (RSD (%)=0.30) and intermediate precision (RSD (%)=0.36) estimates and by Horrat value (0.07). A detailed study of method precision using a nested design demonstrated that variation sources such as instruments, operators and time did not interfere in the variability of results within laboratory and consequently in its intermediate precision. The developed method is environmentally friendly, fast, cheap and easy to implement resulting in an attractive alternative for corn syrups quality control in industries and official laboratories. Copyright © 2017 Elsevier Ltd. All rights reserved.

Complexation equilibria and spectrophotometric determination of iron(III) with 1-amino-4-hydroxyanthraquinone.

PubMed

Abu-Bakr, M S; Sedaira, H; Hashem, E Y

1994-10-01

The complex equilibria of iron(III) with 1-amino-4-hydroxyanthraquinone (AMHA) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaClO(4)). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance-pH graphs. A simple, rapid, selective and sensitive method for the spectrophotometric determination of trace amounts of Fe(III) is developed based on the formation of Fe(AMHA) complex at pH 2.5 (lambda(max) = 640 nm, epsilon approximately = 2.1 x 10(4) L. mol(-1) . cm(-1)) in the presence of a large number of foreign ions. Interferences caused by palladium(II) was masked by the addition of cyanide ions. The method has been applied to the determination of iron in some synthetic samples and polymetallic iron ores.

Comparative Validation of the Determination of Sofosbuvir in Pharmaceuticals by Several Inexpensive Ecofriendly Chromatographic, Electrophoretic, and Spectrophotometric Methods.

PubMed

El-Yazbi, Amira F

2017-01-20

Sofosbuvir (SOFO) was approved by the U.S. Food and Drug Administration in 2013 for the treatment of hepatitis C virusinfection with enhanced antiviral potency compared with earlier analogs. Notwithstanding, all current editions of the pharmacopeias still do not present any analytical methods for the quantification of SOFO. Thus, rapid, simple, and ecofriendly methods for the routine analysis of commercial formulations of SOFO are desirable. In this study, five accurate methods for the determination of SOFO in pharmaceutical tablets were developed and validated. These methods include HPLC, capillary zone electrophoresis, HPTLC, and UV spectrophotometric and derivative spectrometry methods. The proposed methods proved to be rapid, simple, sensitive, selective, and accurate analytical procedures that were suitable for the reliable determination of SOFO in pharmaceutical tablets. An analysis of variance test with <em>P</em>-value &#x003E; 0.05 confirmed that there were no significant differences between the proposed assays. Thus, any of these methods can be used for the routine analysis of SOFO in commercial tablets.

[A new method for the preparation of potassium ferrate and spectroscopic characterization].

PubMed

Zheng, Huai-li; Deng, Lin-li; Ji, Fang-ying; Jiang, Shao-jie; Zhang, Peng

2010-10-01

Calcium hypochlorite was used as the raw material for preparation of the high purity potassium ferrate. The study includes the effects of reaction temperature, recrystallization temperature, reaction time, Ca(ClO)2 dosage, and the amount of calcium hypochlorite on the yield. It was determined that when the reaction temperature was 25 degrees C, recrystallization temperature 0 degree C and reaction time 40 min, the yield was more than 75%. The purity was detected by direct spectrophotometric method to be more than 92%. The product was characterized by infrated spectrum(IR), X-ray diffraction (XRD) and ultraviolet spectrum (UV) methods and proved to be potassium ferrate that was prepared by calcium hypochlorite as the raw material.

Validation of a spectrophotometric procedure for determining nitrate in water samples

USDA-ARS?s Scientific Manuscript database

A single-reagent spectrophotometric procedure using vanadium (III) chloride (VCl3) was found to provide accurate and robust measurement of low levels of nitrate (lNO3-N) in agricultural runoff. Results of the VCl3 method produced data that correlated well (r=0.86; p<0.001) with NO3-N concentrations ...

Utility of N-Bromosuccinimide for the Titrimetric and Spectrophotometric Determination of Famotidine in Pharmaceutical Formulations

PubMed Central

Zenita, O.; Basavaiah, K.

2011-01-01

Two titrimetric and two spectrophotometric methods are described for the assay of famotidine (FMT) in tablets using N-bromosuccinimide (NBS). The first titrimetric method is direct in which FMT is titrated directly with NBS in HCl medium using methyl orange as indicator (method A). The remaining three methods are indirect in which the unreacted NBS is determined after the complete reaction between FMT and NBS by iodometric back titration (method B) or by reacting with a fixed amount of either indigo carmine (method C) or neutral red (method D). The method A and method B are applicable over the range of 2–9 mg and 1–7 mg, respectively. In spectrophotometric methods, Beer's law is obeyed over the concentration ranges of 0.75–6.0 μg mL−1 (method C) and 0.3–3.0 μg mL−1 (method D). The applicability of the developed methods was demonstrated by the determination of FMT in pure drug as well as in tablets. PMID:21760785

Simultaneous determination of piracetam and vincamine by spectrophotometric and high-performance liquid chromatographic methods.

PubMed

El-Saharty, Yasser Shaker Ibrahim

2008-01-01

A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 10-45 and 2-14 microg/mL with mean recoveries of 99.22 +/- 0.72 and 99.67 +/- 0.79%, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 5-45 and 2-14 microg/mL, with mean recoveries of 100.33 +/- 0.54 and 100.44 +/- 0.98% for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphate-methanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5-100 and 2-200 microg/mL, with mean recoveries of 99.62 +/- 0.67 and 99.32 +/- 0.85% for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

Genome-wide comparison of ultraviolet and ethyl methanesulphonate mutagenesis methods for the brown alga Ectocarpus.

PubMed

Godfroy, Olivier; Peters, Akira F; Coelho, Susana M; Cock, J Mark

2015-12-01

Ectocarpus has emerged as a model organism for the brown algae and a broad range of genetic and genomic resources are being generated for this species. The aim of the work presented here was to evaluate two mutagenesis protocols based on ultraviolet irradiation and ethyl methanesulphonate treatment using genome resequencing to measure the number, type and distribution of mutations generated by the two methods. Ultraviolet irradiation generated a greater number of genetic lesions than ethyl methanesulphonate treatment, with more than 400 mutations being detected in the genome of the mutagenised individual. This study therefore confirms that the ultraviolet mutagenesis protocol is suitable for approaches that require a high density of mutations, such as saturation mutagenesis or Targeting Induced Local Lesions in Genomes (TILLING). Copyright © 2015 Elsevier B.V. All rights reserved.

Validation of UV spectrophotometric methods for the determination of dothiepin hydrochloride in pharmaceutical dosage form and stress degradation studies

NASA Astrophysics Data System (ADS)

Abdulrahman, Sameer A. M.; Basavaiah, K.; Cijo, M. X.; Vinay, K. B.

2012-11-01

Spectrophotometric methods have been developed for the determination of dothiepin hydrochloride (DOTH) in both pure and tablet dosage form and their limits of detection and quantification have been evaluated. The methods are based on the measurement of the absorbance of a DOTH solution either in 0.1 N HCl at 229 nm (method A) or in methanol at 231 nm (method B). Beer's law is obeyed over a concentration range of 1-16 μg/ml DOTH for both methods. Molar absorptivity values are calculated to be 2.48 × 104 and 2.42 × 104 l/(mol × cm) with Sandell sensitivity values of 0.0134 and 0.0137 μg/cm2 for methods A and B, respectively. The degradation behavior of DOTH was investigated under different stress conditions such as acid hydrolysis, alkaline hydrolysis, water hydrolysis, oxidation, dry heat treatment, and UV-degradation. The drug undergoes significant degradation under oxidative conditions only.

A comparative study of novel spectrophotometric methods based on isosbestic points; application on a pharmaceutical ternary mixture

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Saleh, Sarah S.; Hassan, Nagiba Y.; Salem, Hesham

This work represents the application of the isosbestic points present in different absorption spectra. Three novel spectrophotometric methods were developed, the first method is the absorption subtraction method (AS) utilizing the isosbestic point in zero-order absorption spectra; the second method is the amplitude modulation method (AM) utilizing the isosbestic point in ratio spectra; and third method is the amplitude summation method (A-Sum) utilizing the isosbestic point in derivative spectra. The three methods were applied for the analysis of the ternary mixture of chloramphenicol (CHL), dexamethasone sodium phosphate (DXM) and tetryzoline hydrochloride (TZH) in eye drops in the presence of benzalkonium chloride as a preservative. The components at the isosbestic point were determined using the corresponding unified regression equation at this point with no need for a complementary method. The obtained results were statistically compared to each other and to that of the developed PLS model. The specificity of the developed methods was investigated by analyzing laboratory prepared mixtures and the combined dosage form. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed.

New simple spectrophotometric method for determination of the binary mixtures (atorvastatin calcium and ezetimibe; candesartan cilexetil and hydrochlorothiazide) in tablets

PubMed Central

Belal, Tarek S.; Daabees, Hoda G.; Abdel-Khalek, Magdi M.; Mahrous, Mohamed S.; Khamis, Mona M.

2012-01-01

A new simple spectrophotometric method was developed for the determination of binary mixtures without prior separation. The method is based on the generation of ratio spectra of compound X by using a standard spectrum of compound Y as a divisor. The peak to trough amplitudes between two selected wavelengths in the ratio spectra are proportional to concentration of X without interference from Y. The method was demonstrated by determination of two drug combinations. The first consists of the two antihyperlipidemics: atorvastatin calcium (ATV) and ezetimibe (EZE), and the second comprises the antihypertensives: candesartan cilexetil (CAN) and hydrochlorothiazide (HCT). For mixture 1, ATV was determined using 10 μg/mL EZE as the divisor to generate the ratio spectra, and the peak to trough amplitudes between 231 and 276 nm were plotted against ATV concentration. Similarly, by using 10 μg/mL ATV as divisor, the peak to trough amplitudes between 231 and 276 nm were found proportional to EZE concentration. Calibration curves were linear in the range 2.5–40 μg/mL for both drugs. For mixture 2, divisor concentration was 7.5 μg/mL for both drugs. CAN was determined using its peak to trough amplitudes at 251 and 277 nm, while HCT was estimated using the amplitudes between 251 and 276 nm. The measured amplitudes were linearly correlated to concentration in the ranges 2.5–50 and 1–30 μg/mL for CAN and HCT, respectively. The proposed spectrophotometric method was validated and successfully applied for the assay of both drug combinations in several laboratory-prepared mixtures and commercial tablets. PMID:29403805

Semi-empirical spectrophotometric (SESp) method for the indirect determination of the ratio of cationic micellar binding constants of counterions X⁻ and Br⁻(K(X)/K(Br)).

PubMed

Khan, Mohammad Niyaz; Yusof, Nor Saadah Mohd; Razak, Norazizah Abdul

2013-01-01

The semi-empirical spectrophotometric (SESp) method, for the indirect determination of ion exchange constants (K(X)(Br)) of ion exchange processes occurring between counterions (X⁻ and Br⁻) at the cationic micellar surface, is described in this article. The method uses an anionic spectrophotometric probe molecule, N-(2-methoxyphenyl)phthalamate ion (1⁻), which measures the effects of varying concentrations of inert inorganic or organic salt (Na(v)X, v = 1, 2) on absorbance, (A(ob)) at 310 nm, of samples containing constant concentrations of 1⁻, NaOH and cationic micelles. The observed data fit satisfactorily to an empirical equation which gives the values of two empirical constants. These empirical constants lead to the determination of K(X)(Br) (= K(X)/K(Br) with K(X) and K(Br) representing cationic micellar binding constants of counterions X and Br⁻). This method gives values of K(X)(Br) for both moderately hydrophobic and hydrophilic X⁻. The values of K(X)(Br), obtained by using this method, are comparable with the corresponding values of K(X)(Br), obtained by the use of semi-empirical kinetic (SEK) method, for different moderately hydrophobic X. The values of K(X)(Br) for X = Cl⁻ and 2,6-Cl₂C6H₃CO₂⁻, obtained by the use of SESp and SEK methods, are similar to those obtained by the use of other different conventional methods.

Two different spectrophotometric determinations of potential anticancer drug and its toxic metabolite.

PubMed

Farid, Nehal F; Abdelwahab, Nada S

2015-06-15

Flutamide is a hormone therapy used for men with advanced prostate cancer. Flutamide is highly susceptible to hydrolysis with the production of 3-(trifluoromethyl)aniline, which is reported to be one of its toxic metabolites, impurities and related substances according to BP and USP. Flutamide was found to be stable when exposed to oxidation by 30% hydrogen peroxide and direct sunlight for up to 4h. Two accurate and sensitive spectrophotometric methods were used for determination of flutamide in bulk and in pharmaceutical formulations. Method (I) is the area under curve (AUC) spectrophotometric method that depends on measuring the AUC in the wavelength ranges of 275-305 nm and 350-380nm and using Cramer's rule. The linearity range was found to be 1-35 μg/mL and 0.5-16 μg/mL for the drug and the degradate, respectively. In method (II), combination of the isoabsorptive and dual wavelength spectrophotometric methods was used for resolving the binary mixture. The absorbance at 249.2 nm (λiso) was used for determination of total mixture concentration, while the difference in absorbance between 232 nm and 341.2 nm was used for measuring the drug concentration. By subtraction, the degradate concentration was obtained. Beer's law was obeyed in the range of 2-35 μg/mL and 0.5-20 μg/mL for the drug and its degradate, respectively. The two methods were validated according to USP guidelines and were applied for determination of the drug in its pharmaceutical dosage form. Moreover AUC method was used for the kinetic study of the hydrolytic degradation of flutamide. The kinetic degradation of flutamide was found to follow pseudo-first order kinetics and is pH and temperature dependent. Activation energy, kinetic rate constants and t1/2 at different temperatures and pH values were calculated. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of new spectrophotometric ratio H-point standard addition method and application to gastrointestinal acting drugs mixtures.

PubMed

Yehia, Ali M

2013-05-15

New, simple, specific, accurate and precise spectrophotometric technique utilizing ratio spectra is developed for simultaneous determination of two different binary mixtures. The developed ratio H-point standard addition method (RHPSAM) was managed successfully to resolve the spectral overlap in itopride hydrochloride (ITO) and pantoprazole sodium (PAN) binary mixture, as well as, mosapride citrate (MOS) and PAN binary mixture. The theoretical background and advantages of the newly proposed method are presented. The calibration curves are linear over the concentration range of 5-60 μg/mL, 5-40 μg/mL and 4-24 μg/mL for ITO, MOS and PAN, respectively. Specificity of the method was investigated and relative standard deviations were less than 1.5. The accuracy, precision and repeatability were also investigated for the proposed method according to ICH guidelines. Copyright © 2013 Elsevier B.V. All rights reserved.

Spectrophotometric calibration procedures to enable calibration-free measurements of seawater calcium carbonate saturation states.

PubMed

Cuyler, Erin E; Byrne, Robert H

2018-08-22

A simple protocol was developed to measure seawater calcium carbonate saturation states (Ω spec ) spectrophotometrically. Saturation states are typically derived from the separate measurement of two other carbon system parameters, with each requiring unique instrumentation and often complex measurement protocols. Using the new protocol, the only required equipment is a thermostatted laboratory spectrophotometer. For each seawater sample, spectrophotometric measurements of pH (visible absorbance) are made in paired optical cells, one with and one without added nitric acid. Ultraviolet absorbance is measured to determine the amount of added acid based on the direct proportionality between nitrate concentration and UV absorbance. Coupled measurements of pH and the alkalinity change that accompanies the nitric acid addition allow calculation of a seawater sample's original carbonate ion concentration and saturation state. These paired absorbance measurements yield Ω spec (and other carbonate system parameters), with each sample requiring about 12 min processing time. Initially, an instrument-specific nitrate molar absorptivity coefficient must be determined (due to small but significant discrepancies in instrumental wavelength calibrations), but thereafter no further calibration is needed. In this work, the 1σ precision of replicate measurements of aragonite saturation state was found to be 0.020, and the average difference between Ω spec and Ω calculated conventionally from measured total alkalinity and pH (Ω calc ) was -0.11% ± 0.96% (a level of accuracy comparable to that obtained from spectrophotometric measurements of carbonate ion concentration). Over the entire range of experimental conditions, 0.97 < Ω < 3.17 (n = 125), all measurements attained the Global Ocean Acidification Observing Network's "weather level" goal for accuracy and 90% attained the more stringent "climate level" goal. When Ω spec was calculated from averages of duplicate

Spectrophotometric analyses of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in water.

PubMed

Shi, Cong; Xu, Zhonghou; Smolinski, Benjamin L; Arienti, Per M; O'Connor, Gregory; Meng, Xiaoguang

2015-07-01

A simple and accurate spectrophotometric method for on-site analysis of royal demolition explosive (RDX) in water samples was developed based on the Berthelot reaction. The sensitivity and accuracy of an existing spectrophotometric method was improved by: replacing toxic chemicals with more stable and safer reagents; optimizing the reagent dose and reaction time; improving color stability; and eliminating the interference from inorganic nitrogen compounds in water samples. Cation and anion exchange resin cartridges were developed and used for sample pretreatment to eliminate the effect of ammonia and nitrate on RDX analyses. The detection limit of the method was determined to be 100 μg/L. The method was used successfully for analysis of RDX in untreated industrial wastewater samples. It can be used for on-site monitoring of RDX in wastewater for early detection of chemical spills and failure of wastewater treatment systems. Copyright © 2015. Published by Elsevier B.V.

Stability-indicating spectrophotometric methods for determination of the anticoagulant drug apixaban in the presence of its hydrolytic degradation product

NASA Astrophysics Data System (ADS)

Tantawy, Mahmoud A.; El-Ragehy, Nariman A.; Hassan, Nagiba Y.; Abdelkawy, Mohamed

2016-04-01

Apixaban (a novel anticoagulant agent) was subjected to a stress stability study including acid, alkali, oxidative, photolytic, and thermal degradation. The drug was found to be only liable to acidic and alkaline hydrolysis. The degradation product was then isolated and identified by IR and GC-mass spectrometry. Four spectrophotometric methods, namely; first derivative (D1), derivative ratio (DR), ratio difference (RD) and mean centering of ratio spectra (MCR), have been suggested for the determination of apixaban in presence of its hydrolytic degradation product. The proposed methods do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated as per ICH guidelines and the specificity was assessed by analyzing synthetic mixtures containing different percentages of the degradation product with the drug. The developed methods were successfully applied for the determination of apixaban in bulk powder and its tablet dosage form.

Stability-indicating spectrophotometric methods for determination of the anticoagulant drug apixaban in the presence of its hydrolytic degradation product.

PubMed

Tantawy, Mahmoud A; El-Ragehy, Nariman A; Hassan, Nagiba Y; Abdelkawy, Mohamed

2016-04-15

Apixaban (a novel anticoagulant agent) was subjected to a stress stability study including acid, alkali, oxidative, photolytic, and thermal degradation. The drug was found to be only liable to acidic and alkaline hydrolysis. The degradation product was then isolated and identified by IR and GC-mass spectrometry. Four spectrophotometric methods, namely; first derivative (D(1)), derivative ratio (DR), ratio difference (RD) and mean centering of ratio spectra (MCR), have been suggested for the determination of apixaban in presence of its hydrolytic degradation product. The proposed methods do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated as per ICH guidelines and the specificity was assessed by analyzing synthetic mixtures containing different percentages of the degradation product with the drug. The developed methods were successfully applied for the determination of apixaban in bulk powder and its tablet dosage form. Copyright © 2016 Elsevier B.V. All rights reserved.

Sensitized spectrophotometric determination of Cr(III) ion for speciation of chromium ion in surfactant media using alpha-benzoin oxime.

PubMed

Ghaedi, Mehrorang; Asadpour, Enayat; Vafaie, Azam

2006-01-01

A simple and accurate micellanized spectrophotometric method for determination of trace amounts of Cr(III) ion in tab and top water and a synthetic mixture has been described. The micellar method is based on effect of organized molecular assemblies such as micelles in spectrophotometric measurement due to their effect on the systems of interest. The ability of micellar system in solubilizing of sparingly soluble ligand or complexes has been used for increasing figures of merit of an analytical method. Due to solubility increasing in aqueous media requirement for a primary extraction can be eliminated. Using the alpha-benzoin oxime (alpha-BO) spectrophotometric determination of Cr(III) ion has been performed and results are compared. The spectrophotometric determination of Cr(III) ion using alpha-BO in the presence of non-ionic surfactant Triton X-100 has been performed. The influence of type and amount of surfactant, pH, complexation time and amount of ligand were examined. Finally, the repeatability, accuracy and the effect of interfering ions on the determination of Cr(III) ion was evaluated. The proposed methods successfully with recovery yield of almost 100% have been applied to the rapid and simple determination of Cr(III) ion in the real samples. There is a good agreement between methods and atomic absorption spectrometry. The Beers law is obeyed over the concentration range of 0.1-13.7 microg mL(-1) for micellar media. The detection limit is 0.8 ng mL(-1). The molar absorptivity of complex is 5350 L mol(-1) cm(-1).

Sensitized spectrophotometric determination of Cr(III) ion for speciation of chromium ion in surfactant media using α-benzoin oxime

NASA Astrophysics Data System (ADS)

Ghaedi, Mehrorang; Asadpour, Enayat; Vafaie, Azam

2006-01-01

A simple and accurate micellanized spectrophotometric method for determination of trace amounts of Cr(III) ion in tab and top water and a synthetic mixture has been described. The micellar method is based on effect of organized molecular assemblies such as micelles in spectrophotometric measurement due to their effect on the systems of interest. The ability of micellar system in solubilizing of sparingly soluble ligand or complexes has been used for increasing figures of merit of an analytical method. Due to solubility increasing in aqueous media requirement for a primary extraction can be eliminated. Using the α-benzoin oxime (α-BO) spectrophotometric determination of Cr(III) ion has been performed and results are compared. The spectrophotometric determination of Cr(III) ion using α-BO in the presence of non-ionic surfactant Triton X-100 has been performed. The influence of type and amount of surfactant, pH, complexation time and amount of ligand were examined. Finally, the repeatability, accuracy and the effect of interfering ions on the determination of Cr(III) ion was evaluated. The proposed methods successfully with recovery yield of almost 100% have been applied to the rapid and simple determination of Cr(III) ion in the real samples. There is a good agreement between methods and atomic absorption spectrometry. The Beers law is obeyed over the concentration range of 0.1-13.7 μg mL-1 for micellar media. The detection limit is 0.8 ng mL-1. The molar absorptivity of complex is 5350 L mol-1 cm-1.

Improving solar ultraviolet irradiance measurements by applying a temperature correction method for Teflon diffusers.

PubMed

Jäkel, Evelyn; den Outer, Peter N; Tax, Rick B; Görts, Peter C; Reinen, Henk A J M

2007-07-10

To establish trends in surface ultraviolet radiation levels, accurate and stable long-term measurements are required. The accuracy level of today's measurements has become high enough to notice even smaller effects that influence instrument sensitivity. Laboratory measurements of the sensitivity of the entrance optics have shown a decrease of as much as 0.07-0.1%/deg temperature increase. Since the entrance optics can heat to greater than 45 degrees C in Dutch summers, corrections are necessary. A method is developed to estimate the entrance optics temperatures from pyranometer measurements and meteorological data. The method enables us to correct historic data records for which temperature information is not available. The temperature retrieval method has an uncertainty of less than 2.5 degrees C, resulting in a 0.3% uncertainty in the correction to be performed. The temperature correction improves the agreement between modeled and measured doses and instrument intercomparison as performed within the Quality Assurance of Spectral Ultraviolet Measurements in Europe project. The retrieval method is easily transferable to other instruments.

Optimization and validation of spectrophotometric methods for determination of finasteride in dosage and biological forms

PubMed Central

Amin, Alaa S.; Kassem, Mohammed A.

2012-01-01

Aim and Background: Three simple, accurate and sensitive spectrophotometric methods for the determination of finasteride in pure, dosage and biological forms, and in the presence of its oxidative degradates were developed. Materials and Methods: These methods are indirect, involve the addition of excess oxidant potassium permanganate for method A; cerric sulfate [Ce(SO4)2] for methods B; and N-bromosuccinimide (NBS) for method C of known concentration in acid medium to finasteride, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of methylene blue for method A, chromotrope 2R for method B, and amaranth for method C at a suitable maximum wavelength, λmax: 663, 528, and 520 nm, for the three methods, respectively. The reaction conditions for each method were optimized. Results: Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.12–3.84 μg mL–1 for method A, and 0.12–3.28 μg mL–1 for method B and 0.14 – 3.56 μg mL–1 for method C. The apparent molar absorptivity, Sandell sensitivity, detection and quantification limits were evaluated. The stoichiometric ratio between the finasteride and the oxidant was estimated. The validity of the proposed methods was tested by analyzing dosage forms and biological samples containing finasteride with relative standard deviation ≤ 0.95. Conclusion: The proposed methods could successfully determine the studied drug with varying excess of its oxidative degradation products, with recovery between 99.0 and 101.4, 99.2 and 101.6, and 99.6 and 101.0% for methods A, B, and C, respectively. PMID:23781478

Efficient flow injection and sequential injection methods for spectrophotometric determination of oxybenzone in sunscreens based on reaction with Ni(II).

PubMed

Chisvert, A; Salvador, A; Pascual-Martí, M C; March, J G

2001-04-01

Spectrophotometric determination of a widely used UV-filter, such as oxybenzone, is proposed. The method is based on the complexation reaction between oxybenzone and Ni(II) in ammoniacal medium. The stoichiometry of the reaction, established by the Job method, was 1:1. Reaction conditions were studied and the experimental parameters were optimized, for both flow injection (FI) and sequential injection (SI) determinations, with comparative purposes. Sunscreen formulations containing oxybenzone were analyzed by the proposed methods and results compared with those obtained by HPLC. Data show that both FI and SI procedures provide accurate and precise results. The ruggedness, sensitivity and LOD are adequate to the analysis requirements. The sample frequency obtained by FI is three-fold higher than that of SI analysis. SI is less reagent-consuming than FI.

Intra-laboratory validation of microplate methods for total phenolic content and antioxidant activity on polyphenolic extracts, and comparison with conventional spectrophotometric methods.

PubMed

Bobo-García, Gloria; Davidov-Pardo, Gabriel; Arroqui, Cristina; Vírseda, Paloma; Marín-Arroyo, María R; Navarro, Montserrat

2015-01-01

Total phenolic content (TPC) and antioxidant activity (AA) assays in microplates save resources and time, therefore they can be useful to overcome the fact that the conventional methods are time-consuming, labour intensive and use large amounts of reagents. An intra-laboratory validation of the Folin-Ciocalteu microplate method to measure TPC and the 2,2-diphenyl-1-picrylhydrazyl (DPPH) microplate method to measure AA was performed and compared with conventional spectrophotometric methods. To compare the TPC methods, the confidence intervals of a linear regression were used. In the range of 10-70 mg L(-1) of gallic acid equivalents (GAE), both methods were equivalent. To compare the AA methodologies, the F-test and t-test were used in a range from 220 to 320 µmol L(-1) of Trolox equivalents. Both methods had homogeneous variances, and the means were not significantively different. The limits of detection and quantification for the TPC microplate method were 0.74 and 2.24 mg L(-1) GAE and for the DPPH 12.07 and 36.58 µmol L(-1) of Trolox equivalents. The relative standard deviation of the repeatability and reproducibility for both microplate methods were ≤ 6.1%. The accuracy ranged from 88% to 100%. The microplate and the conventional methods are equals in a 95% confidence level. © 2014 Society of Chemical Industry.

Accurate quantification of astaxanthin from Haematococcus crude extract spectrophotometrically

NASA Astrophysics Data System (ADS)

Li, Yeguang; Miao, Fengping; Geng, Yahong; Lu, Dayan; Zhang, Chengwu; Zeng, Mingtao

2012-07-01

The influence of alkali on astaxanthin and the optimal working wave length for measurement of astaxanthin from Haematococcus crude extract were investigated, and a spectrophotometric method for precise quantification of the astaxanthin based on the method of Boussiba et al. was established. According to Boussiba's method, alkali treatment destroys chlorophyll. However, we found that: 1) carotenoid content declined for about 25% in Haematococcus fresh cysts and up to 30% in dry powder of Haematococcus broken cysts after alkali treatment; and 2) dimethyl sulfoxide (DMSO)-extracted chlorophyll of green Haematococcus bares little absorption at 520-550 nm. Interestingly, a good linear relationship existed between absorbance at 530 nm and astaxanthin content, while an unknown interference at 540-550 nm was detected in our study. Therefore, with 530 nm as working wavelength, the alkali treatment to destroy chlorophyll was not necessary and the influence of chlorophyll, other carotenoids, and the unknown interference could be avoided. The astaxanthin contents of two samples were measured at 492 nm and 530 nm; the measured values at 530 nm were 2.617 g/100 g and 1.811 g/100 g. When compared with the measured values at 492 nm, the measured values at 530 nm decreased by 6.93% and 11.96%, respectively. The measured values at 530 nm are closer to the true astaxanthin contents in the samples. The data show that 530 nm is the most suitable wave length for spectrophotometric determination to the astaxanthin in Haematococcus crude extract.

Simultaneous determination of atorvastatin calcium and olmesartan medoxomil in a pharmaceutical formulation by reversed phase high-performance liquid chromatography, high-performance thin-layer chromatography, and UV spectrophotometric methods.

PubMed

Soni, Hiral; Kothari, Charmy; Khatri, Deepak; Mehta, Priti

2014-01-01

Validated RP-HPLC, HPTLC, and UV spectrophotometric methods have been developed for the simultaneous determination of atorvastatin calcium (ATV) and olmesartan medoxomil (OLM) in a pharmaceutical formulation. The RP-HPLC separation was achieved on a Kromasil C18 column (250 x 4.6 mm, 5 microm particle size) using 0.01 M potassium dihydrogen o-phosphate (pH 4 adjusted with o-phosphoric acid)-acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1.5 mL/min. Quantification was achieved by UV detection at 276 nm. The HPTLC separation was achieved on precoated silica gel 60F254 plates using chloroform-methanol-acetonitrile (4 + 2+ 4, v/v/v) mobile phase. Quantification was achieved with UV detection at 276 nm. The UV-Vis spectrophotometric method was based on the simultaneous equation method that involves measurement of absorbance at two wavelengths, i.e., 255 nm (lambda max of OLM) and 246.2 nm (lambda max of ATV) in methanol. All three methods were validated as per International Conference on Harmonization guidelines. The proposed methods were simple, precise, accurate, and applicable for the simultaneous determination of ATV and OLM in a marketed formulation. The results obtained by applying the proposed methods were statistically analyzed and were found satisfactory.

Development of an underwater in-situ spectrophotometric sensor for seawater pH

NASA Astrophysics Data System (ADS)

Waterbury, Robert D.; Byrne, Robert H.; Kelly, John; Leader, Bram; McElligott, Sean; Russell, Randy

1996-12-01

A pH sensor based upon spectrophotometric techniques has been developed for in-situ analysis of surface seawater. This sensor utilizes a spectrophotometric pH indicator (Thymol Blue) which has been calibrated for use in seawater as a function of temperature and salinity. Shipboard spectrophotometric pH analyses routinely demonstrate a precision on the order of plus or minus 0.0004 pH units. In- situ analysis of seawater pH has demonstrated a precision on the order of plus or minus 0.001 and an accuracy, using shipboard measurements as a standard, on the order of plus or minus 0.01. The sensor is a self-contained system which pumps seawater, meters in indicator, spectrophotometrically determines indicator absorbance and stores data with a 1 Hz acquisition frequency. The sensor employs two absorbance cells, each with three wavelength channels, to obtain the spectrophotometric absorbance. The sensor system, rated for depths up to 500 m, provides pH, conductivity, temperature and can be operated via computer or in a standalone mode with internal data storage. The sensor utilizes less than 12 watts of power and is packaged in a 29' long by 4.5' diameter aluminum housing.

Detection of latent fingerprints by ultraviolet spectral imaging

NASA Astrophysics Data System (ADS)

Huang, Wei; Xu, Xiaojing; Wang, Guiqiang

2013-12-01

Spectral imaging technology research is becoming more popular in the field of forensic science. Ultraviolet spectral imaging technology is an especial part of the full spectrum of imaging technology. This paper finished the experiment contents of the ultraviolet spectrum imaging method and image acquisition system based on ultraviolet spectral imaging technology. Ultraviolet spectral imaging experiments explores a wide variety of ultraviolet reflectance spectra of the object material curve and its ultraviolet spectrum of imaging modalities, can not only gives a reference for choosing ultraviolet wavelength to show the object surface potential traces of substances, but also gives important data for the ultraviolet spectrum of imaging technology development.

Spectrophotometric determination of isopropamide iodide and trifluoperazine hydrochloride in presence of trifluoperazine oxidative degradate.

PubMed

Abbas, Samah S; Zaazaa, Hala E; Abdelkawy, M; Abdelrahman, Maha M

2010-04-01

Four sensitive, selective and precise stability indicating methods for the determination of isopropamide iodide (ISO) and trifluoperazine hydrochloride (TPZ) in their binary mixture and in presence of trifluoperazine oxidative degradate (OXD). Method A is a derivative spectrophotometric one, where ISO was determined by first derivative (D(1)) at 226.4 nm while TPZ was determined by second derivative (D(2)) at 270.2 nm. Method B is the first derivative of the ratio spectra (DD(1)) spectrophotometric method, ISO can be determined by measuring the peak amplitude at 227.4 nm using 5 microg mL(-1) of OXD as a divisor, while TPZ can be determined by measuring the peak amplitude at 249.2 and 261.4 nm using 15 microg mL(-1) of ISO as a divisor. Method C is the isoabsorptive spectrophotometric method. This method allows determination of ISO and TPZ in their binary mixture by measuring total concentration of ISO and TPZ at their isoabsorptive point at lambda(229.8) nm (Aiso1) while TPZ concentration alone can be determined at lambda(max) 311.2 nm, then ISO concentration can be determined by subtraction. On the same basis TPZ can be determined in presence of ISO and OXD, where OXD concentration alone was determined by measuring the peak amplitude at lambda(281.6) and lambda(309.4) nm while total concentration of TPZ and OXD was determined at their isoabsorptive points at (Aiso2 = 270.2 nm), (Aiso3 = 310.6 nm) and (Aiso4 = 331.8 nm) then TPZ concentration was determined by subtraction. Method D is the multivariate calibration techniques [the classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS)], using the information contained in the absorption spectra of ISO, TPZ and OXD mixtures. The selectivity of the proposed methods was checked using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of ISO and TPZ in pharmaceutical dosage form without interference from other dosage form

Novel ratio difference at coabsorptive point spectrophotometric method for determination of components with wide variation in their absorptivities.

PubMed

Saad, Ahmed S; Abo-Talib, Nisreen F; El-Ghobashy, Mohamed R

2016-01-05

Different methods have been introduced to enhance selectivity of UV-spectrophotometry thus enabling accurate determination of co-formulated components, however mixtures whose components exhibit wide variation in absorptivities has been an obstacle against application of UV-spectrophotometry. The developed ratio difference at coabsorptive point method (RDC) represents a simple effective solution for the mentioned problem, where the additive property of light absorbance enabled the consideration of the two components as multiples of the lower absorptivity component at certain wavelength (coabsorptive point), at which their total concentration multiples could be determined, whereas the other component was selectively determined by applying the ratio difference method in a single step. Mixture of perindopril arginine (PA) and amlodipine besylate (AM) figures that problem, where the low absorptivity of PA relative to AM hinders selective spectrophotometric determination of PA. The developed method successfully determined both components in the overlapped region of their spectra with accuracy 99.39±1.60 and 100.51±1.21, for PA and AM, respectively. The method was validated as per the USP guidelines and showed no significant difference upon statistical comparison with reported chromatographic method. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous Spectrophotometric Estimation of Nitazoxanide and Ofloxacin in Tablets

PubMed Central

Game, Madhuri D.; Sakarkar, D. M.

2011-01-01

Two simple, accurate and precise spectrophotometric methods have been developed for simultaneous determination of nitazoxanide and ofloxacin in tablets. Method I is Q-absorbance ratio method which involves Q-absorbance at isobestic point (306.25 nm) and max (347.5 nm) of nitazoxanide, while method II is two wavelength method, where 244.6 nm and 273.0 nm were selected as 1 and 2 for determination of nitazoxanide and 294.3 nm and 388.1 nm were selected as 3 and 4 for determination of ofloxacin. Both drugs obeyed the Beer's law in the concentration range 2-30 μg/ml,correlation coefficient (r2<1). Both methods were validated statistically and recovery studies were carried out to confirm the accuracy. Commercial tablet formulation was successfully analyzed using the developed methods. PMID:22131624

Spectro-photometric determinations of Mn, Fe and Cu in aluminum master alloys

NASA Astrophysics Data System (ADS)

Rehan; Naveed, A.; Shan, A.; Afzal, M.; Saleem, J.; Noshad, M. A.

2016-08-01

Highly reliable, fast and cost effective Spectro-photometric methods have been developed for the determination of Mn, Fe & Cu in aluminum master alloys, based on the development of calibration curves being prepared via laboratory standards. The calibration curves are designed so as to induce maximum sensitivity and minimum instrumental error (Mn 1mg/100ml-2mg/100ml, Fe 0.01mg/100ml-0.2mg/100ml and Cu 2mg/100ml-10mg/ 100ml). The developed Spectro-photometric methods produce accurate results while analyzing Mn, Fe and Cu in certified reference materials. Particularly, these methods are suitable for all types of Al-Mn, Al-Fe and Al-Cu master alloys (5%, 10%, 50% etc. master alloys).Moreover, the sampling practices suggested herein include a reasonable amount of analytical sample, which truly represent the whole lot of a particular master alloy. Successive dilution technique was utilized to meet the calibration curve range. Furthermore, the workout methods were also found suitable for the analysis of said elements in ordinary aluminum alloys. However, it was observed that Cush owed a considerable interference with Fe, the later one may not be accurately measured in the presence of Cu greater than 0.01 %.

Spectrophotometric Methods for Simultaneous Determination of Sofosbuvir and Ledipasvir (HARVONI Tablet): Comparative Study with Two Generic Products.

PubMed

Abo-Talib, Nisreen F; El-Ghobashy, Mohamed R; Tammam, Marwa H

2017-07-01

Sofosbuvir and ledipasvir are the first drugs in a combination pill to treat chronic hepatitis C virus. Simple, sensitive, and rapid spectrophotometric methods are presented for the determination of sofosbuvir and ledipasvir in their combined dosage form. These methods were based on direct measurement of ledipasvir at 333 nm (due to the lack of interference of sofosbuvir) over a concentration range of 4.0-14.0 µg/mL, with a mean recovery of 100.78 ± 0.64%. Sofosbuvir was determined, without prior separation, by third-derivative values at 281 nm; derivative ratio values at 265.8 nm utilizing 5.0 µg/mL ledipasvir as a divisor; the ratio difference method using values at 270 and 250 nm using 5.0 µg/mL ledipasvir as a divisor; and the ratio subtraction method using values at 261 nm. These methods were found to be linear for sofosbuvir over a concentration range of 5.0-35.0 µg/mL. The suggested methods were validated according to International Conference on Harmonization guidelines. Statistical analysis of the results showed no significant difference between the proposed methods and the manufacturer's LC method of determination with respect to accuracy and precision. These methods were used to compare the equivalence of an innovator drug dosage form and two generic drug dosage forms of the same strength.

A rapid and high-throughput microplate spectrophotometric method for field measurement of nitrate in seawater and freshwater.

PubMed

Wu, Jiapeng; Hong, Yiguo; Guan, Fengjie; Wang, Yan; Tan, Yehui; Yue, Weizhong; Wu, Meilin; Bin, Liying; Wang, Jiaping; Wen, Jiali

2016-02-01

The well-known zinc-cadmium reduction method is frequently used for determination of nitrate. However, this method is seldom to be applied on field research of nitrate due to the long time consuming and large sample volume demand. Here, we reported a modified zinc-cadmium reduction method (MZCRM) for measurement of nitrate at natural-abundance level in both seawater and freshwater. The main improvements of MZCRM include using small volume disposable tubes for reaction, a vortex apparatus for shaking to increase reduction rate, and a microplate reader for high-throughput spectrophotometric measurements. Considering salt effect, two salinity sections (5~10 psu and 20~35 psu) were set up for more accurate determination of nitrate in low and high salinity condition respectively. Under optimized experimental conditions, the reduction rates were stabilized on 72% and 63% on the salinity of 5 and 20 psu respectively. The lowest detection limit for nitrate was 0.5 μM and was linear up to 100 μM (RSDs was 4.8%). Environmental samples assay demonstrated that MZCRM was well consistent with conventional zinc-cadmium reduction method. In total, this modified method improved accuracy and efficiency of operations greatly, and would be realized a rapid and high-throughput determination of nitrate in field analysis of nitrate with low cost.

Thin film optical coatings for the ultraviolet spectral region

NASA Astrophysics Data System (ADS)

Torchio, P.; Albrand, G.; Alvisi, M.; Amra, C.; Rauf, H.; Cousin, B.; Otrio, G.

2017-11-01

The applications and innovations related to the ultraviolet field are today in strong growth. To satisfy these developments which go from biomedical to the large equipment like the Storage Ring Free Electron Laser, it is crucial to control with an extreme precision the optical performances, in using the substrates and the thin film materials impossible to circumvent in this spectral range. In particular, the reduction of the losses by electromagnetic diffusion, Joule effect absorption, or the behavior under UV luminous flows of power, resistance to surrounding particulate flows... become top priority which concerns a broad European and international community. Our laboratory has the theoretical, experimental and technological tools to design and fabricate numerous multilayer coatings with desirable optical properties in the visible and infrared spectral ranges. We have extended our expertise to the ultraviolet. We present here some results on high reflectivity multidielectric mirrors towards 250 nm in wavelength, produced by Ion Plating Deposition. The latter technique allows us to obtain surface treatments with low absorption and high resistance. We give in this study the UV transparent materials and the manufacturing technology which have been the best suited to meet requirements. Single UV layers were deposited and characterized. HfO2/SiO2 mirrors with a reflectance higher than 99% at 300 nm were obtained. Optical and non-optical characterizations such as UV spectrophotometric measurements, X-Ray Diffraction spectra, Scanning Electron Microscope and Atomic Force Microscope images were performed

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods.

PubMed

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-25

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (2(4)) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL(-1) with detection limit of 6.7 ng mL(-1) (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n=7, c=50 ng mL(-1)). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination. Copyright © 2014. Published by Elsevier B.V.

A newly validated and characterized spectrophotometric method for determination of a three water pollutants metal ions

NASA Astrophysics Data System (ADS)

Mohamed, Marwa E.; Frag, Eman Y. Z.; Mohamed, Mona A.

2018-01-01

A simple, fast and accurate spectrophotometric method had been developed to determine lead (II), chromium (III) and barium (II) ions in pure forms and in spiked water samples using thoron (THO) as a reagent forming colored complexes. It was found that the formed complexes absorbed maximally at 539, 540 and 538 nm for Pb(II)-THO, Cr(III)-THO and Ba(II)-THO complexes, respectively. The optimum experimental conditions for these complexes had been studied carefully. Beer's law was obeyed in the range 1-35, 1-70, and 1-45 μg mL- 1 for Pb (II), Cr(III) and Ba(II) ions with THO reagent, respectively. Different parameters such as linearity, selectivity, recovery, limits of quantification and detection, precision and accuracy were also evaluated in order to validate the proposed method. The results showed that, THO was effective in simultaneous determination of Pb(II), Cr(III) and Ba(III) ions in pure forms and in spiked water samples. Also, the results of the proposed method were compared with that obtained from atomic absorption spectrometry. The isolated solid complexes had been characterized using elemental analysis, X-ray powder diffraction (XRD), IR, mass spectrometry and TD-DFT calculations. Their biological activities were investigated against different types of bacteria and fungi organisms.

Spectrophotometric Determination of Phenolic Antioxidants in the Presence of Thiols and Proteins

PubMed Central

Avan, Aslı Neslihan; Demirci Çekiç, Sema; Uzunboy, Seda; Apak, Reşat

2016-01-01

Development of easy, practical, and low-cost spectrophotometric methods is required for the selective determination of phenolic antioxidants in the presence of other similar substances. As electron transfer (ET)-based total antioxidant capacity (TAC) assays generally measure the reducing ability of antioxidant compounds, thiols and phenols cannot be differentiated since they are both responsive to the probe reagent. In this study, three of the most common TAC determination methods, namely cupric ion reducing antioxidant capacity (CUPRAC), 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt/trolox equivalent antioxidant capacity (ABTS/TEAC), and ferric reducing antioxidant power (FRAP), were tested for the assay of phenolics in the presence of selected thiol and protein compounds. Although the FRAP method is almost non-responsive to thiol compounds individually, surprising overoxidations with large positive deviations from additivity were observed when using this method for (phenols + thiols) mixtures. Among the tested TAC methods, CUPRAC gave the most additive results for all studied (phenol + thiol) and (phenol + protein) mixtures with minimal relative error. As ABTS/TEAC and FRAP methods gave small and large deviations, respectively, from additivity of absorbances arising from these components in mixtures, mercury(II) compounds were added to stabilize the thiol components in the form of Hg(II)-thiol complexes so as to enable selective spectrophotometric determination of phenolic components. This error compensation was most efficient for the FRAP method in testing (thiols + phenols) mixtures. PMID:27529232

Spectrophotometric Determination of Phenolic Antioxidants in the Presence of Thiols and Proteins.

PubMed

Avan, Aslı Neslihan; Demirci Çekiç, Sema; Uzunboy, Seda; Apak, Reşat

2016-08-12

Development of easy, practical, and low-cost spectrophotometric methods is required for the selective determination of phenolic antioxidants in the presence of other similar substances. As electron transfer (ET)-based total antioxidant capacity (TAC) assays generally measure the reducing ability of antioxidant compounds, thiols and phenols cannot be differentiated since they are both responsive to the probe reagent. In this study, three of the most common TAC determination methods, namely cupric ion reducing antioxidant capacity (CUPRAC), 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt/trolox equivalent antioxidant capacity (ABTS/TEAC), and ferric reducing antioxidant power (FRAP), were tested for the assay of phenolics in the presence of selected thiol and protein compounds. Although the FRAP method is almost non-responsive to thiol compounds individually, surprising overoxidations with large positive deviations from additivity were observed when using this method for (phenols + thiols) mixtures. Among the tested TAC methods, CUPRAC gave the most additive results for all studied (phenol + thiol) and (phenol + protein) mixtures with minimal relative error. As ABTS/TEAC and FRAP methods gave small and large deviations, respectively, from additivity of absorbances arising from these components in mixtures, mercury(II) compounds were added to stabilize the thiol components in the form of Hg(II)-thiol complexes so as to enable selective spectrophotometric determination of phenolic components. This error compensation was most efficient for the FRAP method in testing (thiols + phenols) mixtures.

Successive spectrophotometric resolution as a novel technique for the analysis of ternary mixtures of pharmaceuticals

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Tawakkol, Shereen M.; Fahmy, Nesma M.; Shehata, Mostafa A.

2014-03-01

A novel spectrophotometric technique was developed for the simultaneous determination of ternary mixtures, without prior separation steps. This technique was called successive spectrophotometric resolution technique. The technique was based on either the successive ratio subtraction or successive derivative subtraction. The mathematical explanation of the procedure was illustrated. In order to evaluate the applicability of the methods a model data as well as an experimental data were tested. The results from experimental data related to the simultaneous spectrophotometric determination of lidocaine hydrochloride (LH), calcium dobesilate (CD) and dexamethasone acetate (DA); in the presence of hydroquinone (HQ), the degradation product of calcium dobesilate were discussed. The proposed drugs were determined at their maxima 202 nm, 305 nm, 239 nm and 225 nm for LH, CD, DA and HQ respectively; by successive ratio subtraction coupled with constant multiplication method to obtain the zero order absorption spectra, while by applying successive derivative subtraction they were determined at their first derivative spectra at 210 nm for LH, 320 nm or P292-320 for CD, 256 nm or P225-252 for DA and P220-233 for HQ respectively. The calibration curves were linear over the concentration range of 2-20 μg/mL for both LH and DA, 6-50 μg/mL for CD, and 3-40 μg/mL for HQ. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs with no interference from other dosage form additives. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically compared with those of the official BP methods for LH, DA, and CD, and with the official USP method for HQ; using student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.

Spectrophotometric determination of substrate-borne polyacrylamide.

PubMed

Lu, Jianhang; Wu, Laosheng

2002-08-28

Polyacrylamides (PAMs) have wide application in many industries and in agriculture. Scientific research and industrial applications manifested a need for a method that can quantify substrate-borne PAM. The N-bromination method (a PAM analytical technique based on N-bromination of amide groups and spectrophotometric determination of the formed starch-triiodide complex), which was originally developed for determining PAM in aqueous solutions, was modified to quantify substrate-borne PAM. In the modified method, the quantity of substrate-borne PAM was converted to a concentration of starch-triiodide complex in aqueous solution that was then measured by spectrophotometry. The method sensitivity varied with substrates due to sorption of reagents and reaction intermediates on the substrates. Therefore, separate calibration for each substrate was required. Results from PAM samples in sand, cellulose, organic matter burnt soils, and clay minerals showed that this method had good accuracy and reproducibility. The PAM recoveries ranged from 95.8% to 103.7%, and the relative standard deviations (n = 4) were <7.5% in all cases. The optimum range of PAM in each sample is 10-80 microg. The technique can serve as an effective tool in improving PAM application and facilitating PAM-related research.

Shedding light on food fraud: spectrophotometric and spectroscopic methods as a tool against economically motivated adulteration of food

NASA Astrophysics Data System (ADS)

Petronijević, R. B.; Velebit, B.; Baltić, T.

2017-09-01

Intentional modification of food or substitution of food ingredients with the aim of gaining profit is food fraud or economically motivated adulteration (EMA). EMA appeared in the food supply chain, and following the global expansion of the food market, has become a world-scale problem for the global economy. Food frauds have involved oils, milk and meat products, infant formula, honey, juices, spices, etc. New legislation was enacted in the last decade in order to fight EMA. Effective analytical methods for food fraud detection are few and still in development. The majority of the methods in common use today for EMA detection are time consuming and inappropriate for use on the production line or out of the laboratory. The next step in the evolution of analytical techniques to combat food fraud is development of fast, accurate methods applicable using portable or handheld devices. Spectrophotometric and spectroscopic methods combined with chemometric analysis, and perhaps in combination with other rapid physico-chemical techniques, could be the answer. This review discusses some analytical techniques based on spectrophotometry and spectroscopy, which are used to reveal food fraud and EMA.

Spectrophotometric characterization of hemozoin as a malaria biomarker

NASA Astrophysics Data System (ADS)

Silva, Ivo; Lima, Rui; Minas, Graça.; Catarino, Susana O.

2017-08-01

Malaria is a parasitic disease with more than a billion people worldwide at risk of contraction. The disease is predominantly widespread in regions with precarious healthcare conditions and resources. Despite the several available malaria diagnostic methods, only two are predominantly used in the field in malaria-endemic countries: microscopy and rapid diagnostic tests. In this work, an alternative diagnostic system is proposed, based on optical absorption spectrophotometry. The main objective of this paper is the spectrophotometric study of hemozoin as a malaria biomarker, since it is a sub-product of the malaria infection. The optical absorbance of hemoglobin and hemozoin solutions in purified water was measured in the visible spectrum range using a spectrophotometric setup. The results showed main absorbance peaks at 540 nm and 574 nm for hemoglobin, and at 672 nm for hemozoin. The tests performed in aqueous solutions have shown that both hemoglobin and synthetic hemozoin, when alone in solution, were detected by absorbance, with sensitivity of 0.05 g/L, and with a high linearity (R2> 0.92 for all wavelength peaks). Furthermore, it was found that the whole blood and the hemoglobin spectra have similar absorption peaks. By combining whole blood and synthetic hemozoin solutions, it was proved that both the hemozoin and the hemoglobin absorbance peaks could still be detected by spectrophotometry. For instance, in polydimethylsiloxane wells, the proposed method was able to detect hemozoin in whole blood samples for optical paths as low as 3 mm in cylindrical wells, thus proving the capability for this method's miniaturization. With this work, it is possible to conclude that hemozoin is a viable candidate as a biomarker for malaria detection by optical absorption spectrophotometry and also, that an autonomous, fully integrated and low cost miniaturized system, based on such a principle, could provide an efficient diagnosis of malaria.

Spectrophotometric and theoretical studies of the protonation of Allura Red AC and Ponceau 4R

NASA Astrophysics Data System (ADS)

Bevziuk, Kateryna; Chebotarev, Alexander; Snigur, Denys; Bazel, Yaroslav; Fizer, Maksym; Sidey, Vasyl

2017-09-01

The acid-base properties of Allura Red AC and Ponceau 4R azo dyes were investigated by spectrophotometric, potentiometric and tristimulus colourimetry methods. Ionization constants of the functional groups were also found in aqueous solutions of the dyes. It was discovered that the wavelength of the maximum light absorption of Allura Red AC and Ponceau 4R solutions does not change significantly over a wide pH range. As a result, spectrophotometric methods yield little information for assessing the acid-base properties of the dyes. It was shown with a help of the tristimulus colourimetry method that it is possible to determine the ionization constants of the functional groups of the dyes even when there is significant overlap of the absorption bands of the acid-base forms. The basic spectrophotometric characteristics of the main forms of Allura Red AC and Ponceau 4R in water and organic solvents were calculated. The molar absorbance coefficients of azo forms were shown to increase as the dielectric permittivity of the solvent increases. It was determined that in aqueous solution the dyes exist in the azo form over a wide range of acidity - pH 2-12 for Allura Red AC (λmax = 505 nm; ελ = 3.1·104 dm3 mol-1 cm-1) and 1-13 for Ponceau 4R (λmax = 510 nm; ελ = 1.7·10-4 dm3 mol-1 cm-1). The most probable protonation/deprotonation schemes were theoretically determined for Allura Red AC and Ponceau 4R using DFT calculations.

Method for high-precision multi-layered thin film deposition for deep and extreme ultraviolet mirrors

DOEpatents

Ruffner, Judith Alison

1999-01-01

A method for coating (flat or non-flat) optical substrates with high-reflectivity multi-layer coatings for use at Deep Ultra-Violet ("DUV") and Extreme Ultra-Violet ("EUV") wavelengths. The method results in a product with minimum feature sizes of less than 0.10-.mu.m for the shortest wavelength (13.4-nm). The present invention employs a computer-based modeling and deposition method to enable lateral and vertical thickness control by scanning the position of the substrate with respect to the sputter target during deposition. The thickness profile of the sputter targets is modeled before deposition and then an appropriate scanning algorithm is implemented to produce any desired, radially-symmetric thickness profile. The present invention offers the ability to predict and achieve a wide range of thickness profiles on flat or figured substrates, i.e., account for 1/R.sup.2 factor in a model, and the ability to predict and accommodate changes in deposition rate as a result of plasma geometry, i.e., over figured substrates.

Method for high-precision multi-layered thin film deposition for deep and extreme ultraviolet mirrors

DOEpatents

Ruffner, J.A.

1999-06-15

A method for coating (flat or non-flat) optical substrates with high-reflectivity multi-layer coatings for use at Deep Ultra-Violet (DUV) and Extreme Ultra-Violet (EUV) wavelengths. The method results in a product with minimum feature sizes of less than 0.10 [micro]m for the shortest wavelength (13.4 nm). The present invention employs a computer-based modeling and deposition method to enable lateral and vertical thickness control by scanning the position of the substrate with respect to the sputter target during deposition. The thickness profile of the sputter targets is modeled before deposition and then an appropriate scanning algorithm is implemented to produce any desired, radially-symmetric thickness profile. The present invention offers the ability to predict and achieve a wide range of thickness profiles on flat or figured substrates, i.e., account for 1/R[sup 2] factor in a model, and the ability to predict and accommodate changes in deposition rate as a result of plasma geometry, i.e., over figured substrates. 15 figs.

Extraction-spectrophotometric determination of tris(2-chloroethyl)amine using phthaleins.

PubMed

Rozsypal, Tomas; Halamek, Emil

2017-06-01

Procedures for the extraction-spectrophotometric determination of tris(2-chloroethyl)amine, an alkylating agent known as a drug as well as a chemical warfare agent (nitrogen mustard HN-3), with 7 acid-base indicators of a triphenylmethane lactone type, phthaleins, were developed. Representatives of phthaleins without an oxygen bridge (thymolphthalein, o-cresolphthalein, naphtholphthalein) and with an oxygen bridge (fluorescein, 2',7'-dichlorofluorescein, eosin B and eosin Y) were used. The methods were based on the formation of ion pair complexes. Chloroform was used as a non-polar solvent for an extraction. The conditions to determine were optimized for the optimal pH of the buffer and the concentration of a phthalein as a reagent. The dependence on the reaction time in a water phase and the stoichiometry of extraction products were studied. The detection limits and the limits of the determination of separate procedures and conditional extraction constants were determined. Comparison with the spectrophotometric method of the group determination of alkyl halides and acyl halides using alkaline ethanol-water solution of thymolphthalein, the so-called T-135 agent, was conducted. While studying the selectivity, the possible interference of bis(2-chloroethyl)sulphide and 3 nitrogen mustards in the proposed procedures were verified. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Simultaneous determination of some ultraviolet-absorbing chemicals in sunscreen cosmetics using a high-performance liquid chromatography method.

PubMed

Liu, T; Wu, D

2011-10-01

A method of gradient elution high-performance liquid chromatography (HPLC) for simultaneous determination of 11 different ultraviolet-absorbing chemicals of phenylbenzlmldazole sulphonic acid, 4-aminobenzoic acid, benzophenone-4, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl methoxycinnamate, homosalate, ethylhexyl salicylate, methylene bis-benzotriazolyl tetramethylbutyl phenol was developed for the application to sunscreen cosmetic products. In this study, an Agilent SB-C18 analytical column (250 × 4.6 mm, 5 μm) was utilized and methanol, tetrahydrofuran and perchloric acid aqueous solution (0.2 mL HClO(4) + 300 mL H(2)O) were used for gradient elution at a total flow rate of 1.0 mL min(-1). The optimum conditions for 11 different ultraviolet-absorbing chemicals analyses were investigated. All calibration curves showed good linear regression with UV detection (311 nm) within test ranges. The correlation coefficients were better than 0.999 in all cases. The assay was simple, selective, convenient and reproducible and is suitable for the determination of ultraviolet-absorbing chemicals in commercial sunscreen cosmetic products. The use frequency of 11 different ultraviolet absorbents in 100 sunscreen cosmetics was investigated and statistically analysed. The ultraviolet absorbent of maximum use frequency was ethylhexyl methoxycinnamate. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Clothing Protection from Ultraviolet Radiation: A New Method for Assessment.

PubMed

Gage, Ryan; Leung, William; Stanley, James; Reeder, Anthony; Barr, Michelle; Chambers, Tim; Smith, Moira; Signal, Louise

2017-11-01

Clothing modifies ultraviolet radiation (UVR) exposure from the sun and has an impact on skin cancer risk and the endogenous synthesis of vitamin D. There is no standardized method available for assessing body surface area (BSA) covered by clothing, which limits generalizability between study findings. We calculated the body cover provided by 38 clothing items using diagrams of BSA, adjusting the values to account for differences in BSA by age. Diagrams displaying each clothing item were developed and incorporated into a coverage assessment procedure (CAP). Five assessors used the CAP and Lund & Browder chart, an existing method for estimating BSA, to calculate the clothing coverage of an image sample of 100 schoolchildren. Values of clothing coverage, inter-rater reliability and assessment time were compared between CAP and Lund & Browder methods. Both methods had excellent inter-rater reliability (>0.90) and returned comparable results, although the CAP method was significantly faster in determining a person's clothing coverage. On balance, the CAP method appears to be a feasible method for calculating clothing coverage. Its use could improve comparability between sun-safety studies and aid in quantifying the health effects of UVR exposure. © 2017 The American Society of Photobiology.

Protection against ultraviolet radiation by commercial summer clothing: need for standardised testing and labelling

PubMed Central

Gambichler, Thilo; Rotterdam, Sebastian; Altmeyer, Peter; Hoffmann, Klaus

2001-01-01

Background The use of clothing as a means of sun protection has been recommended in recent education campaigns. Contrary to popular opinion, however, some fabrics provide insufficient ultraviolet (UV) protection. Material and methods We investigated 236 apparel textiles of the spring/summer collections 2000 and 2001. In accordance with the forthcoming European standard the UV protection factor (UPF) of the fabrics was determined spectrophotometrically. Results Seventy-eight (33%) fabrics had UPF < 15, 45 (19%) had UPF = or > 15 and < 30, and 113 (48%) had UPF = or > 30 (30+). More than 70% of the wool, polyester, and fabric blends, and only less than 30% of the cotton, linen, and viscose fabrics had UPF values of 30+. Fabrics with black, navy-blue, white, green, or beige colours provided most frequently UPF values of 30+. Conclusions It is difficult for the sun-aware consumer to choose the 'right' garment, with a third of summer clothing providing insufficient UV protection and only half of the fabrics having UPF 30+, the UPF recommended by the European standard. Therefore, apparel summer fabrics should be measured and labelled in accordance with a standard document. PMID:11710968

Spectrophotometric and cytochemical analyses of phosphatase activity in Beta vulgaris L.

PubMed

Pesacreta, T C; Bennett, A B; Lucas, W J

1986-03-01

Spectrophotometric and cytochemical methods were used to investigate the localization and/or the sensitivity of phosphatase activities in aldehyde-fixed beet leaves and membrane fractions. The nonspecific acid phosphatase substrates, p-nitrophenyl phosphate and beta-glycerol phosphate, each exhibited unique spectrophotometric patterns of hydrolysis as a function of pH. Additionally, beta-glycerol phosphatase activity was primarily present on the tonoplast, whereas p-nitrophenyl phosphatase was present on the plasma membrane. Because of the unique pH response of each enzyme and their different localization, we conclude that they cannot be entirely "nonspecific." The spectrophotometric pattern of ATP hydrolysis differed from that of p-nitrophenol phosphate in that it decreased at pH 5.0-5.5 and was greatly inhibited by 10 mM sodium fluoride; however, both activities were on the plasma membrane. Therefore, we conclude that these activities represent either two enzymes or only one enzyme that differs in its ability to hydrolyze these two substrates. Generally, enzymatically produced lead deposits on the plasma membrane of non-vascular cells were as frequent and large as those on phloem cells; frequently, deposits on sieve element plasma membranes were relatively small. We therefore conclude that there is no evidence for the presence of relatively intense ATPase activity on the plasma membrane of phloem cells in beet leaf, in contrast to other species. Studies with membrane fractions indicated that formaldehyde could completely inhibit the inhibitor-sensitive phosphatase activities in mitochondrial and vacuolar fractions while preserving significant activity in the plasma membrane fraction.

Spectrophotometric determination of vanadium and its application to gas-turbine fuel-oils.

PubMed

Banerjee, S; Sinha, B P; Dutta, R K

1975-08-01

A very sensitive spectrophotometric method for the determination of vanadium in furnace oils is described. The intense indigo-blue colour developed by the reaction of vanadium with tannin and thioglycollic acid is measured at a wavelength of 600 nm at pH 4 and obeys Beer's law between 0.5 and 5 ppm vanadium. The method is applicable to gas-turbine fuel-oil and special navy fuel-oils. The common mineral constituents usually present in such oils do not interfere.

Spectrophotometric method for quantitative measuring essential oil in aromatic water and distillate with rose smell

NASA Astrophysics Data System (ADS)

Semenova, E.; Presnyakova, V.; Goncharov, D.; Goncharov, M.; Presnyakova, E.; Presnyakov, S.; Moiseeva, I.; Kolesnikova, S.

2017-01-01

In this connection, we improved the express methods of determining the mixture of volatile aromatic substances by the spectrophotometry of aromatic water and steam distillate of essential oil raw materials (traditional or biotechnological with rose smell). Direct spectrophotometry of distillation water is impossible because it is a colloid of liquid oil and law is not observed. Therefore, it is necessary to dissolve 1 ml of distillate in ethanol in the ratio 1:4, in this case we take real solution with no lipophilic fall-out on the walls of cuvette, also the light absorption law is observed. There are stable maximums in spectrums of studied oils. Optical density of these maximums is a result of summary absorption of terpenoid components (aromatic and monoterpene alcohols, its ethers). Optical density of tested and standard solutions is measured in appropriate wavelengths. Spectrophotometric method of determination of essential oil quantity in aromatic water with rose smell differs with high sensitivity (10-5-10-6 gmol/l) and allows to determine oil concentration from 0,900 to 0,008 mg with an error less than 1%. At that, 1 ml is enough for analysis. It’s expedient to apply this method while operating with small quantity of water distillate in biochemical and biotechnological researches and also as express control for extraction and hydrodistillation of essential oil raw material (rose petals and flowers from different origin, eremothecium cultural liquid etc.).

Simultaneous Estimation of Ofloxacin, Clotrimazole, and Lignocaine Hydrochloride in Their Combined Ear-Drop Formulation by Two Spectrophotometric Methods.

PubMed

Bodiwala, Kunjan; Shah, Shailesh; Patel, Yogini; Prajapati, Pintu; Marolia, Bhavin; Kalyankar, Gajanan

2017-01-01

Two sensitive, accurate, and precise spectrophotometric methods have been developed and validated for the simultaneous estimation of ofloxacin (OFX), clotrimazole (CLZ), and lignocaine hydrochloride (LGN) in their combined dosage form (ear drops) without prior separation. The derivative ratio spectra method (method 1) includes the measurement of OFX and CLZ at zero-crossing points (ZCPs) of each other obtained from the ratio derivative spectra using standard LGN as a divisor, whereas the measurement of LGN at the ZCP of CLZ is obtained from the ratio derivative spectra using standard OFX as a divisor. The double divisor-ratio derivative method (method 2) includes the measurement of each drug at its amplitude in the double divisor-ratio spectra obtained using a standard mixture of the other two drugs as the divisor. Both methods were found to be linear (correlation coefficients of >0.996) over the ranges of 3-15, 10-50, and 20-100 μg/mL for OFX, CLZ, and LGN, respectively; precise (RSD of <2%); and accurate (recovery of >98%) for the estimation of each drug. The developed methods were successfully applied for the estimation of these drugs in a marketed ear-drop formulation. Excipients and other ingredients did not interfere with the estimation of these drugs. Both methods were statistically compared using the t-test.

Development and validation of a spectrophotometric method for the determination of macrolide antibiotics by using 2,4-dinitrophenylhydrazine.

PubMed

Abdelmageed, Osama H

2007-01-01

A simple, novel, sensitive, and specific spectrophotometric method was developed and validated for the determination of azithromycin (AZ), clarithromycin (CLA), and roxithromycin (ROX) in bulk powders and their dosage forms. The proposed method was based on the interaction of any of the cited drugs with 2,4-dinitrophenylhydrazine in the presence of an acid catalyst, followed by treatment with a methanolic solution of potassium hydroxide; an intensely colored chromogen was formed that was measured in dimethylformamide, as the diluting solvent, at 542-545, 523-526, and 539-542 nm for AZ, CLA, and ROX, respectively. All variables affecting the development of the measured chromogens were studied and optimized. Beer's law was obeyed in the concentration ranges of 5-40, 5-35, and 5-35 microg/mL for AZ, CLA, and ROX, respectively, with good correlation coefficients (0.9991-0.9999). The limits of detection for this method ranged from 0.77 to 1.47 microg/mL, and the relative standard deviations were 1.24-1.8%. The proposed method was applied successfully to the determination of the 3 drugs in pure bulk form, tablets, and suspensions without interference from commonly encountered additives. The results compared favorably with those of a previously reported method. The mechanism of the reaction was also studied.

Indirect spectrophotometric determination of traces of bromide in water

USGS Publications Warehouse

Fishman, M. J.; Skougstad, M.W.

1963-01-01

A rapid, accurate, and sensitive indirect spectrophotometric method for the determination of bromide in natural waters is based on the catalytic effect of bromide on the oxidation of iodine to iodate by potassium permanganate in sulfuric acid solution. The method is applicable to concentrations ranging from 1 to 100 ??g. of bromide per liter, but may be modified to extend the concentration range. Most ions commonly occurring in water do not interfere. The standard deviation is 2.9 at bromide concentrations of 100 ??g. per liter and less at lower concentrations. The determination of bromide in samples containing known added amounts gave values ranging from 99 to 105% of the concentration calculated to be present.

Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: application to pharmacokinetic studies.

PubMed

Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

2008-01-01

A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 mug/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 mug/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 mug/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

A selective spectrophotometric method for determination of rosoxacin antibiotic using sodium nitroprusside as a chromogenic reagent

NASA Astrophysics Data System (ADS)

Askal, Hassan F.; Refaat, Ibrahim H.; Darwish, Ibrahim A.; Marzouq, Mostafa A.

2008-04-01

A selective spectrophotometric method for the determination of rosoxacin (ROS), a 4-quinolone antimicrobial agent, has been developed and validated. The method was based on the reaction of ROS with alkaline sodium nitroprusside (SNP) reagent at room temperature forming a red colored chromogen measured at 455 nm. The conditions affecting the reaction (SNP concentration, pH, color-developing time, temperature, diluting solvent and chromogen stability time) were optimized. Under the optimum conditions, good linear relationship ( r = 0.9987) was obtained between the absorbance and the concentration of ROS in the range of 20-50 μg ml -1. The assay limits of detection and quantitation were 2.5 and 8.4 μg ml -1, respectively. The method was successfully applied to the analysis of bulk drug and laboratory-prepared tablets; the mean percentage recoveries were 100.1 ± 0.33 and 101.24 ± 1.28%, respectively. The results were compared favourably with those obtained by the reported method; no significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. The robustness and ruggedness of the method was checked and satisfactory results were obtained. The proposed method was found to be highly selective for ROS among the fluoroquinolone antibiotics. The reaction mechanism was proposed and it proceeded in two steps; the formation of nitroferrocyanide by the action of sodium hydroxide alkalinity on SNP and the subsequent formation of the colored nitrosyl-ROS derivative by the attack at position 6 of ROS.

Spectrophotometric study of the charge-transfer and ion-pair complexation of methamphetamine with some acceptors

NASA Astrophysics Data System (ADS)

Shahdousti, Parvin; Aghamohammadi, Mohammad; Alizadeh, Naader

2008-04-01

The charge-transfer (CT) complexes of methamphetamine (MPA) as a n-donor with several acceptors including bromocresolgreen (BCG), bromocresolpurple (BCP), chlorophenolred (CPR), picric acid (PIC), and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) have been studied spectrophotometrically in chloroform solutions in order to obtain some information about their stoichiometry and stability of complexation. The oscillator strengths, transition dipole moments and resonance energy of the complex in the ground state for all complexes have been calculated. Vertical ionization potential of MPA and electron affinity of acceptors were determined by ab initio calculation. The acceptors were also used to utilize a simple and sensitive extraction-spectrophotometric method for the determination of MPA. The method is based on the formation of 1:1 ion-pair association complexes of MPA with BCG, BCP and PIC in chloroform medium. Beer's plots were obeyed in a general concentration range of 0.24-22 μg ml -1 for the investigated drug with different acceptors. The proposed methods were applied successfully for the determination of MAP in pure and abuse drug with good accuracy and precision.

Vemurafenib skin phototoxicity is indirectly linked to ultraviolet A minimal erythema dose decrease.

PubMed

Brugière, C; Stefan, A; Morice, C; Cornet, E; Moreau, A; Allouche, S; Verneuil, L

2014-12-01

Vemurafenib, an anti-rapidly accelerated fibrosarcoma kinase B (BRAF) molecule, improves survival among patients with metastatic BRAF-mutated melanoma. Photosensitivity, a frequent cutaneous adverse effect induced by vemurafenib, can lead to cessation of treatment. To investigate photosensitivity mechanisms in patients treated with vemurafenib for metastatic melanoma. In a prospective study of 12 patients, photobiological explorations with measurements of ultraviolet A (UVA) minimal erythema dose (MED) and polychromatic MED were performed over 3 days in all 12 patients. UVA MED and polychromatic MED were also assessed for four patients before treatment. We then performed spectrophotometric analyses of (i) serum and faeces in these four patients, before and after introduction of vemurafenib; (ii) the lyophilized form of vemurafenib without excipient added; and (iii) the lyophilized form of vemurafenib added to serum and faeces before treatment. Photosensitivity was present in 92% of the patients. UVA MED was normal before treatment and decreased after treatment, while polychromatic MED remained normal. The same three peaks (210, 260 and 310 nm) were identified in the spectrum for UVB and UVC but not for UVA on spectrophotometric analyses for each condition (lyophilized vemurafenib; serum and faeces after introduction of vemurafenib; and lyophilized vemurafenib added to serum and faeces before treatment). The peaks were different before treatment. Our study confirms that photosensitivity under vemurafenib treatment was a UVA phototoxicity reaction, and our results suggest that a metabolite of vemurafenib rather than the parent molecule is involved in this phototoxicity. © 2014 British Association of Dermatologists.

Stimulation of hair cells with ultraviolet light

NASA Astrophysics Data System (ADS)

Azimzadeh, Julien B.; Fabella, Brian A.; Hudspeth, A. J.

2018-05-01

Hair bundles are specialized organelles that transduce mechanical inputs into electrical outputs. To activate hair cells, physiologists have resorted to mechanical methods of hair-bundle stimulation. Here we describe a new method of hair-bundle stimulation, irradiation with ultraviolet light. A hair bundle illuminated by ultraviolet light rapidly moves towards its tall edge, a motion typically associated with excitatory stimulation. The motion disappears upon tip-link rupture and is associated with the opening of mechanotransduction channels. Hair bundles can be induced to move sinusoidally with oscillatory modulation of the stimulation power. We discuss the implications of ultraviolet stimulation as a novel hair-bundle stimulus.

A simple method for determination of carmine in food samples based on cloud point extraction and spectrophotometric detection.

PubMed

Heydari, Rouhollah; Hosseini, Mohammad; Zarabi, Sanaz

2015-01-01

In this paper, a simple and cost effective method was developed for extraction and pre-concentration of carmine in food samples by using cloud point extraction (CPE) prior to its spectrophotometric determination. Carmine was extracted from aqueous solution using Triton X-100 as extracting solvent. The effects of main parameters such as solution pH, surfactant and salt concentrations, incubation time and temperature were investigated and optimized. Calibration graph was linear in the range of 0.04-5.0 μg mL(-1) of carmine in the initial solution with regression coefficient of 0.9995. The limit of detection (LOD) and limit of quantification were 0.012 and 0.04 μg mL(-1), respectively. Relative standard deviation (RSD) at low concentration level (0.05 μg mL(-1)) of carmine was 4.8% (n=7). Recovery values in different concentration levels were in the range of 93.7-105.8%. The obtained results demonstrate the proposed method can be applied satisfactory to determine the carmine in food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel spectrophotometric methods for simultaneous determination of Amlodipine, Valsartan and Hydrochlorothiazide in their ternary mixture

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Hegazy, Maha A.; Mowaka, Shereen; Mohamed, Ekram Hany

2015-04-01

This work represents a comparative study of two smart spectrophotometric techniques namely; successive resolution and progressive resolution for the simultaneous determination of ternary mixtures of Amlodipine (AML), Hydrochlorothiazide (HCT) and Valsartan (VAL) without prior separation steps. These techniques consist of several consecutive steps utilizing zero and/or ratio and/or derivative spectra. By applying successive spectrum subtraction coupled with constant multiplication method, the proposed drugs were obtained in their zero order absorption spectra and determined at their maxima 237.6 nm, 270.5 nm and 250 nm for AML, HCT and VAL, respectively; while by applying successive derivative subtraction they were obtained in their first derivative spectra and determined at P230.8-246, P261.4-278.2, P233.7-246.8 for AML, HCT and VAL respectively. While in the progressive resolution, the concentrations of the components were determined progressively from the same zero order absorption spectrum using absorbance subtraction coupled with absorptivity factor methods or from the same ratio spectrum using only one divisor via amplitude modulation method can be used for the determination of ternary mixtures using only one divisor where the concentrations of the components are determined progressively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs. Moreover comparative study between spectrum addition technique as a novel enrichment technique and a well established one namely spiking technique was adopted for the analysis of pharmaceutical formulations containing low concentration of AML. The methods were validated as per ICH guidelines where accuracy, precision and specificity were found to be within their acceptable limits. The results obtained from the proposed methods were statistically compared with the reported one where no significant

Application of Certain π-Acceptors for the Spectrophotometric Determination of Alendronate Sodium in Pharmaceutical Bulk and Dosage Forms.

PubMed

Raza, Asad; Zia-Ul-Haq, Muhammad

2011-01-01

Two simple, fast, and accurate spectrophotometric methods for the determination of alendronate sodium are described. The methods are based on charge-transfer complex formation of the drug with two π-electron acceptors 7,7,7,8-tetracyanoquinodimethane (TCNQ) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in acetonitrile and methanol medium. The methods are followed spectrophotometrically by measuring the maximum absorbance at 840 nm and 465 nm, respectively. Under the optimized experimental conditions, the calibration curves showed a linear relationship over the concentration ranges of 2-10 μg mL(-1) and 2-12 μg mL(-1), respectively. The optimal reactions conditions values such as the reagent concentration, heating time, and stability of reaction product were determined. No significant difference was obtained between the results of newly proposed methods and the B.P. Titrimetric procedures. The charge transfer approach using TCNQ and DDQ procedures described in this paper is simple, fast, accurate, precise, and extraction-free.

Liquid chromatographic and spectrophotometric determination of diflucortolone valerate and isoconazole nitrate in creams.

PubMed

Karacan, Elif; Cağlayan, Mehmet Gokhan; Palabiyik, Ismail Murat; Onur, Feyyaz

2011-01-01

A new RP-LC method and two new spectrophotometric methods, principal component regression (PCR) and first derivative spectrophotometry, are proposed for simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) in cream formulations. An isocratic system consisting of an ACE C18 column and a mobile phase composed of methanol-water (95 + 5, v/v) was used for the optimal chromatographic separation. In PCR, the concentration data matrix was prepared by using synthetic mixtures containing these drugs in methanol-water (3 + 1, v/v). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 29 wavelengths in the range of 242-298 nm for DIF and ISO in the zero-order spectra of their combinations. In first derivative spectrophotometry, dA/dlambda values were measured at 247.8 nm for DIF and at 240.2 nm for ISO in first derivative spectra of the solution of DIF and ISO in methanol-water (3 + 1, v/v). The linear ranges were 4.00-48.0 microg/mL for DIF and 50.0-400 microg/mL for ISO in the LC method, and 2.40-40.0 microg/mL for DIF and 60.0-260 microg/mL for ISO in the PCR and first derivative spectrophotometric methods. These methods were validated by analyzing synthetic mixtures. These three methods were successfully applied to two pharmaceutical cream preparations.

Novel spectrophotometric method for determination of some macrolide antibiotics in pharmaceutical formulations using 1,2-naphthoquinone-4-sulphonate

NASA Astrophysics Data System (ADS)

Ashour, Safwan; Bayram, Roula

2012-12-01

New, simple and rapid spectrophotometric method has been developed and validated for the assay of two macrolide drugs, azithromycin (AZT) and erythromycin (ERY) in pure and pharmaceutical formulations. The proposed method was based on the reaction of AZT and ERY with sodium 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline medium at 25 °C to form an orange-colored product of maximum absorption peak at 452 nm. All variables were studied to optimize the reaction conditions and the reaction mechanism was postulated. Beer's law was obeyed in the concentration range 1.5-33.0 and 0.92-8.0 μg mL-1 with limit of detection values of 0.026 and 0.063 μg mL-1 for AZT and ERY, respectively. The calculated molar absorptivity values are 4.3 × 104 and 12.3 × 104 L mol-1 cm-1 for AZT and ERY, respectively. The proposed methods were successfully applied to the determination of AZT and ERY in formulations and the results tallied well with the label claim. The results were statistically compared with those of an official method by applying the Student's t-test and F-test. No interference was observed from the concomitant substances normally added to preparations.

Thoron-tartaric acid systems for spectrophotometric determination of thorium

USGS Publications Warehouse

Grimaldi, F.S.; Fletcher, M.H.

1956-01-01

Thoron is commonly used for the spectrophotometric determination of thorium. An undesirable feature of its use is its high sensitivity to zirconium. This study describes the use of tartaric acid as a masking reagent for zirconium. Three tartaric acid-thoron systems, developed for the determination of thorium, differ with respect to the concentrations of thoron and tartaric acid. Mesotartaric acid, used in one of the systems, is most effective in masking zirconium. The behavior of rarer elements, usually associated with thorium ores, is determined in two systems, and a dilution method is described for the direct determination of thorium in monazite concentrates.

Ultraviolet Extensions

NASA Technical Reports Server (NTRS)

2008-01-01

[figure removed for brevity, see original site] Side-by-Side Comparison Click on image for larger view

This ultraviolet image from NASA's Galaxy Evolution Explorer shows the Southern Pinwheel galaxy, also know as Messier 83 or M83. It is located 15 million light-years away in the southern constellation Hydra.

Ultraviolet light traces young populations of stars; in this image, young stars can be seen way beyond the main spiral disk of M83 up to 140,000 light-years from its center. Could life exist around one of these far-flung stars? Scientists say it's unlikely because the outlying regions of a galaxy are lacking in the metals required for planets to form.

The image was taken at scheduled intervals between March 15 and May 20, 2007. It is one of the longest-exposure, or deepest, images ever taken of a nearby galaxy in ultraviolet light. Near-ultraviolet light (or longer-wavelength ultraviolet light) is colored yellow, and far-ultraviolet light is blue.

What Lies Beyond the Edge of a Galaxy The side-by-side comparison shows the Southern Pinwheel galaxy, or M83, as seen in ultraviolet light (right) and at both ultraviolet and radio wavelengths (left). While the radio data highlight the galaxy's long, octopus-like arms stretching far beyond its main spiral disk (red), the ultraviolet data reveal clusters of baby stars (blue) within the extended arms.

The ultraviolet image was taken by NASA's Galaxy Evolution Explorer between March 15 and May 20, 2007, at scheduled intervals. Back in 2005, the telescope first photographed M83 over a shorter period of time. That picture was the first to reveal far-flung baby stars forming up to 63,000 light-years from the edge of the main spiral disk. This came as a surprise to astronomers because a galaxy's outer territory typically lacks high densities of star-forming materials.

The newest picture of M83 from the Galaxy Evolution Explorer is shown at the right, and was taken over a longer period of

Ion chromatography with the indirect ultraviolet detection of alkali metal ions and ammonium using imidazolium ionic liquid as ultraviolet absorption reagent and eluent.

PubMed

Liu, Yong-Qiang; Yu, Hong

2016-08-01

Indirect ultraviolet detection was conducted in ultraviolet-absorption-agent-added mobile phase to complete the detection of the absence of ultraviolet absorption functional group in analytes. Compared with precolumn derivatization or postcolumn derivatization, this method can be widely used, has the advantages of simple operation and good linear relationship. Chromatographic separation of Li(+) , Na(+) , K(+) , and NH4 (+) was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid/organic solvent as the mobile phase, in which imidazolium ionic liquids acted as ultraviolet absorption reagent and eluting agent. The retention behaviors of four kinds of cations are discussed, and the mechanism of separation and detection are described. The main factors influencing the separation and detection were the background ultraviolet absorption reagent and the concentration of hydrogen ion in the ion chromatography-indirect ultraviolet detection. The successful separation and detection of Li(+) , Na(+) , K(+) , and NH4 (+) within 13 min was achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.02, 0.11, 0.30, and 0.06 mg/L, respectively. A new separation and analysis method of alkali metal ions and ammonium by ion chromatography with indirect ultraviolet detection method was developed, and the application range of ionic liquid was expanded. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HPTLC and Spectrophotometric Estimation of Febuxostat and Diclofenac Potassium in Their Combined Tablets.

PubMed

El-Yazbi, Fawzi A; Amin, Omayma A; El-Kimary, Eman I; Khamis, Essam F; Younis, Sameh E

2016-08-01

An accurate, precise, rapid, specific and economic high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitative determination of febuxostat (FEB) and diclofenac potassium (DIC). The chromatographic separation was performed on precoated silica gel 60 GF254 plates with chloroform-methanol 7:3 (v/v) as the mobile phase. The developed plates were scanned and quantified at 289 nm. Experimental conditions including band size, mobile phase composition and chamber-saturation time were critically studied, and the optimum conditions were selected. A satisfactory resolution (Rs = 2.67) with RF 0.48 and 0.69 and high sensitivity with limits of detection of 4 and 7 ng/band for FEB and DIC, respectively, were obtained. In addition, derivative ratio and ratio difference spectrophotometric methods were established for the analysis of such a mixture. All methods were validated as per the ICH guidelines. In the HPTLC method, the calibration plots were linear between 0.01-0.55 and 0.02-0.60 µg/band, for FEB and DIC, respectively. For the spectrophotometric methods, the calibration graphs were linear between 2-14 and 4-18 µg/mL for FEB and DIC, respectively. The simplicity and specificity of the proposed methods suggest their application in quality control analysis of FEB and DIC in their raw materials and tablets. A comparison of the proposed methods with the existing methods is presented. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A fully battery-powered inexpensive spectrophotometric system for high-sensitivity point-of-care analysis on a microfluidic chip

PubMed Central

Dou, Maowei; Lopez, Juan; Rios, Misael; Garcia, Oscar; Xiao, Chuan; Eastman, Michael

2016-01-01

A cost-effective battery-powered spectrophotometric system (BASS) was developed for quantitative point-of-care (POC) analysis on a microfluidic chip. By using methylene blue as a model analyte, we first compared the performance of the BASS with a commercial spectrophotometric system, and further applied the BASS for loop-mediated isothermal amplification (LAMP) detection and subsequent quantitative nucleic acid analysis which exhibited a comparable limit of detection to that of Nanodrop. Compared to the commercial spectrophotometric system, our spectrophotometric system is lower-cost, consumes less reagents, and has a higher detection sensitivity. Most importantly, it does not rely on external power supplies. All these features make our spectrophotometric system highly suitable for a variety of POC analyses, such as field detection. PMID:27143408

Novel Atomic Absorption Spectrometric and Rapid Spectrophotometric Methods for the Quantitation of Paracetamol in Saliva: Application to Pharmacokinetic Studies

PubMed Central

Issa, M. M.; Nejem, R. M.; El-Abadla, N. S.; Al-Kholy, M.; Saleh, Akila. A.

2008-01-01

A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 μg/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 μg/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 μg/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%. PMID:20046743

A PLS-based extractive spectrophotometric method for simultaneous determination of carbamazepine and carbamazepine-10,11-epoxide in plasma and comparison with HPLC

NASA Astrophysics Data System (ADS)

Hemmateenejad, Bahram; Rezaei, Zahra; Khabnadideh, Soghra; Saffari, Maryam

2007-11-01

Carbamazepine (CBZ) undergoes enzyme biotransformation through epoxidation with the formation of its metabolite, carbamazepine-10,11-epoxide (CBZE). A simple chemometrics-assisted spectrophotometric method has been proposed for simultaneous determination of CBZ and CBZE in plasma. A liquid extraction procedure was operated to separate the analytes from plasma, and the UV absorbance spectra of the resultant solutions were subjected to partial least squares (PLS) regression. The optimum number of PLS latent variables was selected according to the PRESS values of leave-one-out cross-validation. A HPLC method was also employed for comparison. The respective mean recoveries for analysis of CBZ and CBZE in synthetic mixtures were 102.57 (±0.25)% and 103.00 (±0.09)% for PLS and 99.40 (±0.15)% and 102.20 (±0.02)%. The concentrations of CBZ and CBZE were also determined in five patients using the PLS and HPLC methods. The results showed that the data obtained by PLS were comparable with those obtained by HPLC method.

Spectrophotometric determination of triclosan in personal care products

NASA Astrophysics Data System (ADS)

Lu, Huihui; Ma, Hongbing; Tao, Guanhong

2009-09-01

A spectrophotometric method for the determination of triclosan in personal care products was proposed. It was based on the reaction of sodium nitrite with p-sulfanilic acid in an acidic medium to form diazonium ion, with which triclosan further formed an azo compound in an alkaline medium. The resulting yellow colored product has a maximum absorption at 452 nm. A good linear relationship ( r = 0.9999) was obtained in the range of 0-30 mg L -1 triclosan. A detection limit of 0.079 g L -1 was achieved and the relative standard deviation was 0.24% ( n = 11) at 14 mg L -1 triclosan. The proposed method has been applied to the analyses of triclosan in several personal care products and the results were in good agreement with those obtained by high-performance liquid chromatography.

Photoresist composition for extreme ultraviolet lithography

DOEpatents

Felter, T. E.; Kubiak, G. D.

1999-01-01

A method of producing a patterned array of features, in particular, gate apertures, in the size range 0.4-0.05 .mu.m using projection lithography and extreme ultraviolet (EUV) radiation. A high energy laser beam is used to vaporize a target material in order to produce a plasma which in turn, produces extreme ultraviolet radiation of a characteristic wavelength of about 13 nm for lithographic applications. The radiation is transmitted by a series of reflective mirrors to a mask which bears the pattern to be printed. The demagnified focused mask pattern is, in turn, transmitted by means of appropriate optics and in a single exposure, to a substrate coated with photoresists designed to be transparent to EUV radiation and also satisfy conventional processing methods. A photoresist composition for extreme ultraviolet radiation of boron carbide polymers, hydrochlorocarbons and mixtures thereof.

Sensitive inexpensive spectrophotometric and spectrofluorimetric analysis of ezogabine, levetiracetam and topiramate in tablet formulations using Hantzsch condensation reaction

NASA Astrophysics Data System (ADS)

Ibrahim, F. A.; El-Yazbi, A. F.; Wagih, M. M.; Barary, M. A.

2017-09-01

Two highly sensitive, simple and selective spectrophotometric and spectrofluorimetric assays have been investigated for the analysis of ezogabine, levetiracetam and topiramate in their pure and in pharmaceutical dosage forms. The suggested methods depend on the condensation of the primary amino-groups in the three drugs with acetylacetone and formaldehyde according to Hantzsch reaction yielding highly fluorescent yellow colored dihydropyridine derivatives. The reaction products of ezogabine, levetiracetam and topiramate were measured spectrophotometrically at 418, 390 and 380 nm or spectrofluorimetrically at λem/ex of 495/425 nm, 490/415 nm and 488/410 nm, respectively. Various experimental conditions have been carefully studied to maximize the reaction yield. At the optimum reaction conditions, the calibration curves were rectilinear over the concentration ranges of 8-25, 60-180 and 80-200 μg/mL spectrophotometrically and 0.02-0.2, 0.2-1.2 and 0.2-1.5 μg/mL spectrofluorimetrically for ezogabine, levetiracetam and topiramate, respectively with good correlation coefficients. The suggested methods were applied successfully for the analysis of ezogabine, levetiracetam and topiramate in their commercial tablets with high percentage recoveries and negligible interference from various excipients in pharmaceutical dosage forms. The results were statistically analyzed and showed the absence of any significant difference between both developed and published methods. The procedures were validated and evaluated by the ICH guidelines revealing good reproducibility and accuracy. Therefore, the two proposed methods may be considered of high interest for practical and reliable analysis of ezogabine, levetiracetam and topiramate in pharmaceutical dosage forms.

Spectrophotometric total reducing sugars assay based on cupric reduction.

PubMed

Başkan, Kevser Sözgen; Tütem, Esma; Akyüz, Esin; Özen, Seda; Apak, Reşat

2016-01-15

As the concentration of reducing sugars (RS) is controlled by European legislation for certain specific food and beverages, a simple and sensitive spectrophotometric method for the determination of RS in various food products is proposed. The method is based on the reduction of Cu(II) to Cu(I) with reducing sugars in alkaline medium in the presence of 2,9-dimethyl-1,10-phenanthroline (neocuproine: Nc), followed by the formation of a colored Cu(I)-Nc charge-transfer complex. All simple sugars tested had the linear regression equations with almost equal slope values. The proposed method was successfully applied to fresh apple juice, commercial fruit juices, milk, honey and onion juice. Interference effect of phenolic compounds in plant samples was eliminated by a solid phase extraction (SPE) clean-up process. The method was proven to have higher sensitivity and precision than the widely used dinitrosalicylic acid (DNS) colorimetric method. Copyright © 2015 Elsevier B.V. All rights reserved.

The Hopkins Ultraviolet Telescope - Performance and calibration during the Astro-1 mission

NASA Technical Reports Server (NTRS)

Davidsen, Arthur F.; Long, Knox S.; Durrance, Samuel T.; Blair, William P.; Bowers, Charles W.; Conard, Steven J.; Feldman, Paul D.; Ferguson, Henry C.; Fountain, Glen H.; Kimble, Randy A.

1992-01-01

Results are reported of spectrophotometric observations, made with the Hopkins Ultraviolet Telescope (HUT), of 77 astronomical sources throughout the far-UV (912-1850 A) at a resolution of about 3 A, and, for a small number of sources, in the extreme UV (415-912 A) beyond the Lyman limit at a resolution of about 1.5 A. The HUT instrument and its performance in orbit are described. A HUT observation of the DA white dwarf G191-B2B is presented, and the photometric calibration curve for the instrument is derived from a comparison of the observation with a model stellar atmosphere. The sensitivity reaches a maximum at 1050 A, where 1 photon/sq cm s A yields 9.5 counts/s A, and remains within a factor of 2 of this value from 912 to 1600 A. The instrumental dark count measured on orbit was less than 0.001 counts/s A.

Development of a quantitative assessment method of pigmentary skin disease using ultraviolet optical imaging.

PubMed

Lee, Onseok; Park, Sunup; Kim, Jaeyoung; Oh, Chilhwan

2017-11-01

The visual scoring method has been used as a subjective evaluation of pigmentary skin disorders. Severity of pigmentary skin disease, especially melasma, is evaluated using a visual scoring method, the MASI (melasma area severity index). This study differentiates between epidermal and dermal pigmented disease. The study was undertaken to determine methods to quantitatively measure the severity of pigmentary skin disorders under ultraviolet illumination. The optical imaging system consists of illumination (white LED, UV-A lamp) and image acquisition (DSLR camera, air cooling CMOS CCD camera). Each camera is equipped with a polarizing filter to remove glare. To analyze images of visible and UV light, images are divided into frontal, cheek, and chin regions of melasma patients. Each image must undergo image processing. To reduce the curvature error in facial contours, a gradient mask is used. The new method of segmentation of front and lateral facial images is more objective for face-area-measurement than the MASI score. Image analysis of darkness and homogeneity is adequate to quantify the conventional MASI score. Under visible light, active lesion margins appear in both epidermal and dermal melanin, whereas melanin is found in the epidermis under UV light. This study objectively analyzes severity of melasma and attempts to develop new methods of image analysis with ultraviolet optical imaging equipment. Based on the results of this study, our optical imaging system could be used as a valuable tool to assess the severity of pigmentary skin disease. © 2017 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Indirect spectrophotometric determination of arbutin, whitening agent through oxidation by periodate and complexation with ferric chloride

NASA Astrophysics Data System (ADS)

Barsoom, B. N.; Abdelsamad, A. M. E.; Adib, N. M.

2006-07-01

A simple and accurate spectrophotometric method for the determination of arbutin (glycosylated hydroquinone) is described. It is based on the oxidation of arbutin by periodate in presence of iodate. Excess periodate causes liberation of iodine at pH 8.0. The unreacted periodate is determined by measurement of the liberated iodine spectrophotometrically in the wavelength range (300-500 nm). A calibration curve was constructed for more accurate results and the correlation coefficient of linear regression analysis was -0.9778. The precision of this method was better than 6.17% R.S.D. ( n = 3). Regression analysis of Bear-Lambert plot shows good correlation in the concentration range 25-125 ug/ml. The identification limit was determined to be 25 ug/ml a detailed study of the reaction conditions was carried out, including effect of changing pH, time, temperature and volume of periodate. Analyzing pure and authentic samples containing arbutin tested the validity of the proposed method which has an average percent recovery of 100.86%. An alternative method is also proposed which involves a complexation reaction between arbutin and ferric chloride solution. The produced complex which is yellowish-green in color was determined spectophotometrically.

Spectrophotometric Quantification of Flavonoids in Herbal Material, Crude Extract, and Fractions from Leaves of Eugenia uniflora Linn.

PubMed

Ramos, Rhayanne T M; Bezerra, Isabelle C F; Ferreira, Magda R A; Soares, Luiz Alberto Lira

2017-01-01

The traditional use of Eugenia uniflora L. ("Pitanga") is reported due to several properties, which have often been related to its flavonoid content. The aim was to evaluate analytical procedures for quantification of total flavonoids content (TFCs) by ultraviolet-visible (UV-Vis) spectrophotometry in the herbal material (HM), crude extract (CE), and fractions from leaves of E. uniflora . The method for quantification of flavonoids after complexation with aluminum chloride (AlCl 3 ) was evaluated: amount of sample (0.25-1.5 g); solvent (40%-80% ethanol); reaction time and AlCl 3 concentration (2.5%-7.5%). The procedures by direct dilution (DD) and after acid hydrolysis (AH) were used and validated for HM and CE and applied to the aqueous fraction (AqF), hexane fraction, and ethyl acetate fractions (EAF). The ideal conditions of analysis were ethanol 80% as solvent; 0.5 g of sample; λmax of 408 (DD) and 425 nm (AH); 25 min after addition of AlCl 3 5%. The procedures validated for standards and samples showed linearity ( R 2 > 0.99) with limit of detection and limit of quantification between 0.01 and 0.17 mg/mL (rutin and quercetin); and 0.03 and 0.09 mg/mL (quercetin), for DD and AH, respectively. The procedures were accurate (detect, practice, and repair < 5% and recovery >90%), and stable under robustness conditions (luminosity, storage, reagents, and equipment). The TFCs in AqF and EAF were 0.65 g% and 17.72 g%, calculated as rutin. UV-Vis methods for quantification of TFC in HM, CE, and fractions from leaves of E. uniflora were suitably validated. Regarding the analysis of fractions, the EAF achieved enrichment of about nine times in the content of flavonoids. The total flavonoids content (TFCs) of herbal material, crude extract, and fractions from Eugenia uniflora can be quantified by ultraviolet-visibleThe spectrophotometric methods (direct dilution and acid hydrolysis) were reproducible and able to quantify TFC in raw material and derivatives from leaves of

Quantitative HPLC Analysis of Rosmarinic Acid in Extracts of "Melissa officinalis" and Spectrophotometric Measurement of Their Antioxidant Activities

ERIC Educational Resources Information Center

Canelas, Vera; da Costa, Cristina Teixeira

2007-01-01

The students prepare tea samples using different quantities of lemon balm leaves ("Melissa officinalis") and measure the rosmarinic acid contents by an HPLC-DAD method. The antioxidant properties of the tea samples are evaluated by a spectrophotometric method using a radical-scavenging assay with DPPH. (2,2-diphenyl-1-picrylhydrazyl). Finally the…

Spectrophotometric determination of flucloxacillin and dicloxacillin in pure and dosage forms

NASA Astrophysics Data System (ADS)

El-Dien, F. A. Nour; Mohamed, Gehad G.; Farag, Eman Y. Z. A.

2006-05-01

A simple, rapid and accurate spectrophotometric method for the determination of antibiotic drugs, flucloxacillin (Fluclox) and dicloxacillin (Diclox), in pure form and different pharmaceutical preparations has been developed. The charge transfer (CT) reactions between Fluclox and Diclox as electron donors and 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE) as π-acceptors to give highly coloured complex species have been spectrophotometrically studied. The optimum experimental conditions for these CT reactions have been studied carefully. Beer's law is obeyed over the concentration ranges of 4-180 μg mL -1 and 4-70 μg mL -1 for Fluclox and Diclox drugs using TCNQ and TCNE reagents, respectively. The Sandell sensitivities ( S) are found to be 0.016-0.035 μg cm -2 and 0.011-0.016 μg cm -2 for Fluclox and Diclox, respectively, which indicate the high sensitivity of the proposed method. The relative standard deviations (R.S.D.: 0.08-0.49 and 0.15-0.80) for the determination of Fluclox and (R.S.D.: 0.05-0.75 and 0.13-0.75) for Diclox were obtained for four to six replicates using TCNQ and TCNE reagents, respectively, refer to the high accuracy and precision of the proposed method. These results are also confirmed by the between-day precision and the percent recovery of 99.90-100.1 and 99.60-100.4 for Fluclox and 99.90-100.5 and 99.40-100.1 for Diclox using TNCQ and TCNE reagents, respectively. The results obtained for the two reagents are comparable with those obtained by the official method.

Spectrophotometric determination of flucloxacillin and dicloxacillin in pure and dosage forms.

PubMed

El-Dien, F A Nour; Mohamed, Gehad G; Farag, Eman Y Z A

2006-05-01

A simple, rapid and accurate spectrophotometric method for the determination of antibiotic drugs, flucloxacillin (Fluclox) and dicloxacillin (Diclox), in pure form and different pharmaceutical preparations has been developed. The charge transfer (CT) reactions between Fluclox and Diclox as electron donors and 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE) as pi-acceptors to give highly coloured complex species have been spectrophotometrically studied. The optimum experimental conditions for these CT reactions have been studied carefully. Beer's law is obeyed over the concentration ranges of 4-180 microg mL(-1) and 4-70 microg mL(-1) for Fluclox and Diclox drugs using TCNQ and TCNE reagents, respectively. The Sandell sensitivities (S) are found to be 0.016-0.035 microg cm(-2) and 0.011-0.016 microg cm(-2) for Fluclox and Diclox, respectively, which indicate the high sensitivity of the proposed method. The relative standard deviations (R.S.D.: 0.08-0.49 and 0.15-0.80) for the determination of Fluclox and (R.S.D.: 0.05-0.75 and 0.13-0.75) for Diclox were obtained for four to six replicates using TCNQ and TCNE reagents, respectively, refer to the high accuracy and precision of the proposed method. These results are also confirmed by the between-day precision and the percent recovery of 99.90-100.1 and 99.60-100.4 for Fluclox and 99.90-100.5 and 99.40-100.1 for Diclox using TNCQ and TCNE reagents, respectively. The results obtained for the two reagents are comparable with those obtained by the official method.

Spectrophotometric and computerized evaluation of tooth bleaching employing 10 different home-bleaching procedures: In-vitro study

PubMed Central

Peskersoy, Cem; Tetik, Ayhan; Ozturk, Veli Ozgen; Gokay, Necmi

2014-01-01

Objective: The aim of this in-vitro study was to evaluate the efficacy of bleaching products, determine the applicability and validation of the measurement methods. Materials and Methods: Freshly extracted 110 human incisor teeth were stained with whole blood and hemolysate solution prior to the application of 10 different home-bleaching products. Spectrophotometric measurements of the tooth shades were performed for each specimen before and after bleaching at the 1st, 3rd, 7th, and 14 days. Differences in lightness (Δl), chroma (Δc), hue (Δh) values and shade changes were measured to evaluate process. Computerized digital imaging analyses to determine the color changes were performed with Photoshop CS4 software (Adobe, San Jose, CA, USA). Statistical analyses were performed with analysis of variance, Scheffe and Tukey tests. Results: In all of the test groups regardless of the material used, a significant increase in lightness and hue, and decrease of chroma were observed, as compared to the control group. After recommended bleaching applications, Δl and Δh values respectively increased in group Zaris White and Brite (ZWB) and group Pola Night and Δc values showed significant decrease in groups ZWB and Rembrandt REM3 (P < 0.05). At the end of the procedure both spectrophotometric and digital imaging analysis showed ZWB was the most effective product among the others while Yotuel and Happy Smile were the least (P < 0.05). Conclusions: Home-bleaching systems showed slower but almost permanent bleaching effect likewise office-based methods. Both software and spectrophotometric analyses have advantages such as evaluating the results objectively and numerically, also treatment outcomes could be preserved. PMID:25512738

Use of lignin extracted from different plant sources as standards in the spectrophotometric acetyl bromide lignin method.

PubMed

Fukushima, Romualdo S; Kerley, Monty S

2011-04-27

A nongravimetric acetyl bromide lignin (ABL) method was evaluated to quantify lignin concentration in a variety of plant materials. The traditional approach to lignin quantification required extraction of lignin with acidic dioxane and its isolation from each plant sample to construct a standard curve via spectrophotometric analysis. Lignin concentration was then measured in pre-extracted plant cell walls. However, this presented a methodological complexity because extraction and isolation procedures are lengthy and tedious, particularly if there are many samples involved. This work was targeted to simplify lignin quantification. Our hypothesis was that any lignin, regardless of its botanical origin, could be used to construct a standard curve for the purpose of determining lignin concentration in a variety of plants. To test our hypothesis, lignins were isolated from a range of diverse plants and, along with three commercial lignins, standard curves were built and compared among them. Slopes and intercepts derived from these standard curves were close enough to allow utilization of a mean extinction coefficient in the regression equation to estimate lignin concentration in any plant, independent of its botanical origin. Lignin quantification by use of a common regression equation obviates the steps of lignin extraction, isolation, and standard curve construction, which substantially expedites the ABL method. Acetyl bromide lignin method is a fast, convenient analytical procedure that may routinely be used to quantify lignin.

Multi-wavelength spectrophotometric analysis for detection of xanthochromia in cerebrospinal fluid and accuracy for the diagnosis of subarachnoid hemorrhage.

PubMed

Smith, Andrew; Wu, Alan H B; Lynch, Kara L; Ko, Nerissa; Grenache, David G

2013-09-23

Cerebrospinal fluid (CSF) was examined for bilirubin, an important indicator for diagnosis of subarachnoid hemorrhage (SAH). A multi-wavelength (340, 415, and 460 nm) spectrophotometric assay was developed for the quantitative measurement of bilirubin in CSF, enabling the mathematical correction for absorbance of hemoglobin and proteins. Bilirubin and hemoglobin results were correlated to HPLC and a standard colorimetric assay, respectively. A subset of samples was sent for an absorbance reading at 450 nm following baseline correction. The multi-wavelength bilirubin assay was validated on 70 patients with confirmed SAH and 70 patients with neurologic symptoms who ruled out for SAH. The multi-wavelength spectrophometric assay demonstrated no interferences due to proteins (albumin) up to 30 g/l or oxyhemoglobin up to 260 mg/l. The assay limit of detection was 0.2 mg/l, linear to 20 mg/l, and CVs ranged from 1 to 6% at bilirubin concentrations of 0.84 and 2.1mg/l. The spectrophotometric assay correlated to HPLC and the colorimetric assay for bilirubin and hemoglobin, respectively. Results also correlated to the absorbance method (with removal of samples with high hemoglobin and proteins). The area under the ROC curve for diagnosis of SAH was 0.971 and 0.954 for the HPLC and spectrophotometric assay, respectively. At a cutoff of 0.2mg/l, the clinical specificity was 100% for both assays, and the clinical sensitivity was 94.3% and 88.6% for SAH for the HPLC and spectrophotometric asays, respectively. The multi-wavelength spectrophotometric assay is an objective alternative to visual inspection, HPLC, and absorbance for CSF bilirubin. Copyright © 2013 Elsevier B.V. All rights reserved.

A convenient spectrophotometric assay for the determination of l-ergothioneine in blood

PubMed Central

Carlsson, Jan; Kierstan, Marek P. J.; Brocklehurst, Keith

1974-01-01

1. A convenient spectrophotometric assay for the determination of l-ergothioneine in solution including deproteinized blood haemolysate was developed. 2. The method consists of deproteinization by heat precipitation and Cu2+-catalysed oxidation of thiols such as glutathione and of l-ascorbic acid, both in alkaline media, and titration of l-ergothioneine (which is not oxidized under these conditions) by its virtually instantaneous reaction with 2,2′-dipyridyl disulphide at pH1. 3. This method and the results obtained with it for the analysis of human, horse, sheep and pig blood are compared with existing methods of l-ergothioneine analysis and the results obtained thereby. PMID:4463946

Spectrophotometric determination of H2O2-generating oxidases using oxyhemoglobin as oxygen donor and indicator.

PubMed

Bârzu, O; Dânşoreanu, M

1980-01-01

1. Spectrophotometric determination of oxygen uptake using oxyhemoglobin as oxygen donor and indicator was used for assay of H2O2-generating oxidases like monoamine oxidase and glucose oxidase. 2. In order to decompose H2O2 formed during the oxygen uptake, catalase and methanol (or ethanol) was added to the respiratory system. At pH values higher than 7.5 the oxydation of deoxygenated hemoglobin to methemoglobin was less than 3%. 2. Oxidases with low Km for oxygen can be assayed using the spectrophotometric method if suitable correction factors are introduced into the calculation of oxygen uptake. The correction factor represents the ratio of the rate of formation (or disappearance) of one of the reactants and the rate of oxyhemoglobin deoxygenation, measured under identical experimental conditions.

Modeling systematic errors: polychromatic sources of Beer-Lambert deviations in HPLC/UV and nonchromatographic spectrophotometric assays.

PubMed

Galli, C

2001-07-01

It is well established that the use of polychromatic radiation in spectrophotometric assays leads to excursions from the Beer-Lambert limit. This Note models the resulting systematic error as a function of assay spectral width, slope of molecular extinction coefficient, and analyte concentration. The theoretical calculations are compared with recent experimental results; a parameter is introduced which can be used to estimate the magnitude of the systematic error in both chromatographic and nonchromatographic spectrophotometric assays. It is important to realize that the polychromatic radiation employed in common laboratory equipment can yield assay errors up to approximately 4%, even at absorption levels generally considered 'safe' (i.e. absorption <1). Thus careful consideration of instrumental spectral width, analyte concentration, and slope of molecular extinction coefficient is required to ensure robust analytical methods.

Spectrophotometric Study of the Region of the Sky Around the Galaxies Markarian 261 and 262

NASA Astrophysics Data System (ADS)

Khachikian, E. Ye.; Sargsyan, L. A.

2005-10-01

Results are presented from a detailed spectrophotometric study of a unique system of physically coupled galaxies whose spectra contain identical emission lines. This system consists of four galaxies, three of which have a double or multiple structure in their central portions and are, by definition, galaxies with two or multiple nuclei. Two of these objects are the galaxies with an ultraviolet excess (UVE), Mark 261 and Mark 262, while one is a galaxy made up of two identical starlike nuclei that are referred to as the “twin objects.” In the DSS2 charts, the latter show up as two adjacent stars without any surroundings. However, there are two condensations between these starlike nuclei. The fourth object has a triplet structure. It is shown here that all these objects have the same emission (line) spectra and red shifts. All the physical characteristics that can be determined from the spectra are determined: red shifts, relative intensities of emission lines, their equivalent widths, distances to the galaxies, etc. It is concluded that the members of this system have a common origin, more or less consistent with Ambartsumyan's idea of the fragmentation of an isolated, high density body.

Development and Validation of UV-Visible Spectrophotometric Method for Simultaneous Determination of Eperisone and Paracetamol in Solid Dosage Form.

PubMed

Khanage, Shantaram Gajanan; Mohite, Popat Baban; Jadhav, Sandeep

2013-01-01

Eperisone Hydrochloride (EPE) is a potent new generation antispasmodic drug which is used in the treatment of moderate to severe pain in combination with Paracetamol (PAR). Both drugs are available in tablet dosage form in combination with a dose of 50 mg for EPE and 325 mg PAR respectively. The method is based upon Q-absorption ratio method for the simultaneous determination of the EPE and PAR. Absorption ratio method is used for the ratio of the absorption at two selected wavelength one of which is the iso-absorptive point and other being the λmax of one of the two components. EPE and PAR shows their iso-absorptive point at 260 nm in methanol, the second wavelength used is 249 nm which is the λmax of PAR in methanol. The linearity was obtained in the concentration range of 5-25 μg/mL for EPE and 2-10 μg/mL for PAR. The proposed method was effectively applied to tablet dosage form for estimation of both drugs. The accuracy and reproducibility results are close to 100% with 2% RSD. RESULTS of the analysis were validated statistically and found to be satisfactory. The results of proposed method have been validated as per ICH guidelines. A simple, precise and economical spectrophotometric method has been developed for the estimation of EPE and PAR in pharmaceutical formulation.

Application of Certain π-Acceptors for the Spectrophotometric Determination of Alendronate Sodium in Pharmaceutical Bulk and Dosage Forms

PubMed Central

Raza, Asad; Zia-ul-Haq, Muhammad

2011-01-01

Two simple, fast, and accurate spectrophotometric methods for the determination of alendronate sodium are described. The methods are based on charge-transfer complex formation of the drug with two π-electron acceptors 7,7,7,8-tetracyanoquinodimethane (TCNQ) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in acetonitrile and methanol medium. The methods are followed spectrophotometrically by measuring the maximum absorbance at 840 nm and 465 nm, respectively. Under the optimized experimental conditions, the calibration curves showed a linear relationship over the concentration ranges of 2–10 μg mL−1 and 2–12 μg mL−1, respectively. The optimal reactions conditions values such as the reagent concentration, heating time, and stability of reaction product were determined. No significant difference was obtained between the results of newly proposed methods and the B.P. Titrimetric procedures. The charge transfer approach using TCNQ and DDQ procedures described in this paper is simple, fast, accurate, precise, and extraction-free. PMID:21760789

SPECTROPHOTOMETRIC DETERMINATION OF ULTRA-SMALL QUANTITIES OF NICKEL IN INDIUM (in Russian)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peshkova, V.M.; Bochkova, V.M.; Astakhova, E.K.

1961-09-01

alpha -Benzil doxime permits the determination of nickel by measuring optical density in the region of maximum absortption (at 275 m mu ), after the reagent excess is removed by washing the extract with alkali. Conditions were found for the spectrophotometric determination of ultra-small quantities (down to 0.005 gamma ) of nickel with alpha -benzil dioxime in the soultion of its pure salt, in the presence of cobalt and copper. A method was developed for the determination of traces of nickel down to 5 x 10 /sup -7%/ in metallic indium. The reproducibility of method is +25%. (auth)

Improving Assessment of Lifetime Solar Ultraviolet Radiation Exposure in Epidemiologic Studies: Comparison of Ultraviolet Exposure Assessment Methods in a Nationwide United States Occupational Cohort.

PubMed

Little, Mark P; Tatalovich, Zaria; Linet, Martha S; Fang, Michelle; Kendall, Gerald M; Kimlin, Michael G

2018-06-13

Solar ultraviolet radiation is the primary risk factor for skin cancers and sun-related eye disorders. Estimates of individual ambient ultraviolet irradiance derived from ground-based solar measurements and from satellite measurements have rarely been compared. Using self-reported residential history from 67,189 persons in a nationwide occupational US radiologic technologists cohort, we estimated ambient solar irradiance using data from ground-based meters and noontime satellite measurements. The mean distance-moved from city of longest residence in childhood increased from 137.6 km at ages 13-19 to 870.3 km at ages ≥65, with corresponding increases in absolute latitude-difference moved. At ages 20/40/60/80, the Pearson/Spearman correlation coefficients of ground-based and satellite-derived solar potential ultraviolet exposure, using irradiance and cumulative radiant-exposure metrics, were high (=0.87-0.92). There was also moderate correlation (Pearson/Spearman correlation coefficients=0.51-0.60) between irradiance at birth and at last-known address, for ground-based and satellite data. Satellite-based lifetime estimates of ultraviolet radiation were generally 14-15% lower than ground-based estimates, albeit with substantial uncertainties, possibly because ground-based estimates incorporate fluctuations in cloud and ozone, which are incompletely incorporated in the single noontime satellite-overpass ultraviolet value. If confirmed elsewhere, the findings suggest that ground-based estimates may improve exposure-assessment accuracy and potentially provide new insights into ultraviolet-radiation-disease relationships in epidemiologic studies. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

DLLME-spectrophotometric determination of glyphosate residue in legumes.

PubMed

Çetin, Emine; Şahan, Serkan; Ülgen, Ahmet; Şahin, Uğur

2017-09-01

A new separation and pre-concentration method for spectrophotometric determination of glyphosate herbicide was developed. Glyphosate was converted into dithiocarbamic acid with CS 2 , followed by copper in the presence of ammonia to promote complex formation. This complex was collected in a CH 2 Cl 2 organic drop and absorbance measured at 435nm. The analytical parameters, such as the amount of NH 3 , Cu(II) and CS 2 , type of extraction solutions, and the ratio of dispersive and organic liquids were optimized. The calibration curve was linear in the range 0.5-10mgl -1 . The limits of detection and quantification were calculated from 3s to 10s criterions as 0.21mgl -1 and 0.70mgl -1 , respectively. The developed method was applied to legume samples with the satisfactory recovery values of 98±4-102±3%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Research in extreme ultraviolet and far ultraviolet astronomy

NASA Technical Reports Server (NTRS)

Labov, S. E.

1985-01-01

Instruments designed to explore different aspects of far and extreme ultraviolet cosmic radiation were studied. The far ultraviolet imager (FUVI) was flown on the Aries sounding rocket. Its unique large format 75mm detector mapped out the far ultraviolet background radiation with a resolution of only a few arc minutes. Analysis of this data indicates to what extent the FUVI background is extra galactic in origin. A power spectrum of the spatial fluctuations will have direct consequences for galactic evolution.

Development and validation of a UV-spectrophotometric method for the determination of pheniramine maleate and its stability studies

NASA Astrophysics Data System (ADS)

Raghu, M. S.; Basavaiah, K.; Ramesh, P. J.; Abdulrahman, Sameer A. M.; Vinay, K. B.

2012-03-01

A sensitive, precise, and cost-effective UV-spectrophotometric method is described for the determination of pheniramine maleate (PAM) in bulk drug and tablets. The method is based on the measurement of absorbance of a PAM solution in 0.1 N HCl at 264 nm. As per the International Conference on Harmonization (ICH) guidelines, the method was validated for linearity, accuracy, precision, limits of detection (LOD) and quantification (LOQ), and robustness and ruggedness. A linear relationship between absorbance and concentration of PAM in the range of 2-40 μg/ml with a correlation coefficient (r) of 0.9998 was obtained. The LOD and LOQ values were found to be 0.18 and 0.39 μg/ml PAM, respectively. The precision of the method was satisfactory: the value of relative standard deviation (RSD) did not exceed 3.47%. The proposed method was applied successfully to the determination of PAM in tablets with good accuracy and precision. Percentages of the label claims ranged from 101.8 to 102.01% with the standard deviation (SD) from 0.64 to 0.72%. The accuracy of the method was further ascertained by recovery studies via a standard addition procedure. In addition, the forced degradation of PAM was conducted in accordance with the ICH guidelines. Acidic and basic hydrolysis, thermal stress, peroxide, and photolytic degradation were used to assess the stability-indicating power of the method. A substantial degradation was observed during oxidative and alkaline degradations. No degradation was observed under other stress conditions.

Spectrophotometric probe

DOEpatents

Prather, W.S.; O'Rourke, P.E.

1994-08-02

A support structure is described bearing at least one probe for making spectrophotometric measurements of a fluid using a source of light and a spectrophotometer. The probe includes a housing with two optical fibers and a planoconvex lens. A sleeve bearing a mirror surrounds the housing. The lens is separated from the mirror by a fixed distance, defining an interior space for receiving a volume of the fluid sample. A plurality of throughholes extending through the sleeve communicate between the sample volume and the exterior of the probe, all but one hole bearing a screen. A protective jacket surrounds the probe. A hollow conduit bearing a tube is formed in the wall of the probe for venting any air in the interior space when fluid enters. The probe is held at an acute angle so the optic fibers carrying the light to and from the probe are not bent severely on emergence from the probe. 3 figs.

Spectrophotometric probe

DOEpatents

Prather, William S.; O'Rourke, Patrick E.

1994-01-01

A support structure bearing at least one probe for making spectrophotometric measurements of a fluid using a source of light and a spectrophotometer. The probe includes a housing with two optical fibers and a planoconvex lens. A sleeve bearing a mirror surrounds the housing. The lens is separated from the mirror by a fixed distance, defining an interior space for receiving a volume of the fluid sample. A plurality of throughholes extending through the sleeve communicate between the sample volume and the exterior of the probe, all but one hole bearing a screen. A protective jacket surrounds the probe. A hollow conduit bearing a tube is formed in the wall of the probe for venting any air in the interior space when fluid enters. The probe is held at an acute angle so the optic fibers carrying the light to and from the probe are not bent severely on emergence from the probe.

Enhancing prediction power of chemometric models through manipulation of the fed spectrophotometric data: A comparative study

NASA Astrophysics Data System (ADS)

Saad, Ahmed S.; Hamdy, Abdallah M.; Salama, Fathy M.; Abdelkawy, Mohamed

2016-10-01

Effect of data manipulation in preprocessing step proceeding construction of chemometric models was assessed. The same set of UV spectral data was used for construction of PLS and PCR models directly and after mathematically manipulation as per well known first and second derivatives of the absorption spectra, ratio spectra and first and second derivatives of the ratio spectra spectrophotometric methods, meanwhile the optimal working wavelength ranges were carefully selected for each model and the models were constructed. Unexpectedly, number of latent variables used for models' construction varied among the different methods. The prediction power of the different models was compared using a validation set of 8 mixtures prepared as per the multilevel multifactor design and results were statistically compared using two-way ANOVA test. Root mean squares error of prediction (RMSEP) was used for further comparison of the predictability among different constructed models. Although no significant difference was found between results obtained using Partial Least Squares (PLS) and Principal Component Regression (PCR) models, however, discrepancies among results was found to be attributed to the variation in the discrimination power of adopted spectrophotometric methods on spectral data.

A fast and direct spectrophotometric method for the simultaneous determination of methyl paraben and hydroquinone in cosmetic products using successive projections algorithm.

PubMed

Esteki, M; Nouroozi, S; Shahsavari, Z

2016-02-01

To develop a simple and efficient spectrophotometric technique combined with chemometrics for the simultaneous determination of methyl paraben (MP) and hydroquinone (HQ) in cosmetic products, and specifically, to: (i) evaluate the potential use of successive projections algorithm (SPA) to derivative spectrophotometric data in order to provide sufficient accuracy and model robustness and (ii) determine MP and HQ concentration in cosmetics without tedious pre-treatments such as derivatization or extraction techniques which are time-consuming and require hazardous solvents. The absorption spectra were measured in the wavelength range of 200-350 nm. Prior to performing chemometric models, the original and first-derivative absorption spectra of binary mixtures were used as calibration matrices. Variable selected by successive projections algorithm was used to obtain multiple linear regression (MLR) models based on a small subset of wavelengths. The number of wavelengths and the starting vector were optimized, and the comparison of the root mean square error of calibration (RMSEC) and cross-validation (RMSECV) was applied to select effective wavelengths with the least collinearity and redundancy. Principal component regression (PCR) and partial least squares (PLS) were also developed for comparison. The concentrations of the calibration matrix ranged from 0.1 to 20 μg mL(-1) for MP, and from 0.1 to 25 μg mL(-1) for HQ. The constructed models were tested on an external validation data set and finally cosmetic samples. The results indicated that successive projections algorithm-multiple linear regression (SPA-MLR), applied on the first-derivative spectra, achieved the optimal performance for two compounds when compared with the full-spectrum PCR and PLS. The root mean square error of prediction (RMSEP) was 0.083, 0.314 for MP and HQ, respectively. To verify the accuracy of the proposed method, a recovery study on real cosmetic samples was carried out with satisfactory

Experimental evaluation of optimization method for developing ultraviolet barrier coatings

NASA Astrophysics Data System (ADS)

Gonome, Hiroki; Okajima, Junnosuke; Komiya, Atsuki; Maruyama, Shigenao

2014-01-01

Ultraviolet (UV) barrier coatings can be used to protect many industrial products from UV attack. This study introduces a method of optimizing UV barrier coatings using pigment particles. The radiative properties of the pigment particles were evaluated theoretically, and the optimum particle size was decided from the absorption efficiency and the back-scattering efficiency. UV barrier coatings were prepared with zinc oxide (ZnO) and titanium dioxide (TiO2). The transmittance of the UV barrier coating was calculated theoretically. The radiative transfer in the UV barrier coating was modeled using the radiation element method by ray emission model (REM2). In order to validate the calculated results, the transmittances of these coatings were measured by a spectrophotometer. A UV barrier coating with a low UV transmittance and high VIS transmittance could be achieved. The calculated transmittance showed a similar spectral tendency with the measured one. The use of appropriate particles with optimum size, coating thickness and volume fraction will result in effective UV barrier coatings. UV barrier coatings can be achieved by the application of optical engineering.

AN AUTOMATIC DETECTION METHOD FOR EXTREME-ULTRAVIOLET DIMMINGS ASSOCIATED WITH SMALL-SCALE ERUPTION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alipour, N.; Safari, H.; Innes, D. E.

2012-02-10

Small-scale extreme-ultraviolet (EUV) dimming often surrounds sites of energy release in the quiet Sun. This paper describes a method for the automatic detection of these small-scale EUV dimmings using a feature-based classifier. The method is demonstrated using sequences of 171 Angstrom-Sign images taken by the STEREO/Extreme UltraViolet Imager (EUVI) on 2007 June 13 and by Solar Dynamics Observatory/Atmospheric Imaging Assembly on 2010 August 27. The feature identification relies on recognizing structure in sequences of space-time 171 Angstrom-Sign images using the Zernike moments of the images. The Zernike moments space-time slices with events and non-events are distinctive enough to be separatedmore » using a support vector machine (SVM) classifier. The SVM is trained using 150 events and 700 non-event space-time slices. We find a total of 1217 events in the EUVI images and 2064 events in the AIA images on the days studied. Most of the events are found between latitudes -35 Degree-Sign and +35 Degree-Sign . The sizes and expansion speeds of central dimming regions are extracted using a region grow algorithm. The histograms of the sizes in both EUVI and AIA follow a steep power law with slope of about -5. The AIA slope extends to smaller sizes before turning over. The mean velocity of 1325 dimming regions seen by AIA is found to be about 14 km s{sup -1}.« less

A simple spectrophotometric method for determination of zirconium or hafnium in selected molybdenum-base alloys

NASA Technical Reports Server (NTRS)

Dupraw, W. A.

1972-01-01

A simple analytical procedure is described for accurately and precisely determining the zirconium or hafnium content of molybdenum-base alloys. The procedure is based on the reaction of the reagent Arsenazo III with zirconium or hafnium in strong hydrochloric acid solution. The colored complexes of zirconium or hafnium are formed in the presence of molybdenum. Titanium or rhenium in the alloy have no adverse effect on the zirconium or hafnium complex at the following levels in the selected aliquot: Mo, 10 mg; Re, 10 mg; Ti, 1 mg. The spectrophotometric measurement of the zirconium or hafnium complex is accomplished without prior separation with a relative standard deviation of 1.3 to 2.7 percent.

Simultaneous determination of mebeverine hydrochloride and chlordiazepoxide in their binary mixture using novel univariate spectrophotometric methods via different manipulation pathways

NASA Astrophysics Data System (ADS)

Lotfy, Hayam M.; Fayez, Yasmin M.; Michael, Adel M.; Nessim, Christine K.

2016-02-01

Smart, sensitive, simple and accurate spectrophotometric methods were developed and validated for the quantitative determination of a binary mixture of mebeverine hydrochloride (MVH) and chlordiazepoxide (CDZ) without prior separation steps via different manipulating pathways. These pathways were applied either on zero order absorption spectra namely, absorbance subtraction (AS) or based on the recovered zero order absorption spectra via a decoding technique namely, derivative transformation (DT) or via ratio spectra namely, ratio subtraction (RS) coupled with extended ratio subtraction (EXRS), spectrum subtraction (SS), constant multiplication (CM) and constant value (CV) methods. The manipulation steps applied on the ratio spectra are namely, ratio difference (RD) and amplitude modulation (AM) methods or applying a derivative to these ratio spectra namely, derivative ratio (DD1) or second derivative (D2). Finally, the pathway based on the ratio spectra of derivative spectra is namely, derivative subtraction (DS). The specificity of the developed methods was investigated by analyzing the laboratory mixtures and was successfully applied for their combined dosage form. The proposed methods were validated according to ICH guidelines. These methods exhibited linearity in the range of 2-28 μg/mL for mebeverine hydrochloride and 1-12 μg/mL for chlordiazepoxide. The obtained results were statistically compared with those of the official methods using Student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.

A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection

NASA Astrophysics Data System (ADS)

Riad, Safaa M.; El-Rahman, Mohamed K. Abd; Fawaz, Esraa M.; Shehata, Mostafa A.

2015-06-01

Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 μg/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

Simultaneous Determination of Octinoxate, Oxybenzone, and Octocrylene in a Sunscreen Formulation Using Validated Spectrophotometric and Chemometric Methods.

PubMed

Abdel-Ghany, Maha F; Abdel-Aziz, Omar; Ayad, Miriam F; Mikawy, Neven N

2015-01-01

Accurate, reliable, and sensitive spectrophotometric and chemometric methods were developed for simultaneous determination of octinoxate (OMC), oxybenzone (OXY), and octocrylene (OCR) in a sunscreen formulation without prior separation steps, including derivative ratio spectra zero crossing (DRSZ), double divisor ratio spectra derivative (DDRD), mean centering ratio spectra (MCR), and partial least squares (PLS-2). With the DRSZ technique, the UV filters could be determined in the ranges of 0.5-13.0, 0.3-9.0, and 0.5-9.0 μg/mL at 265.2, 246.6, and 261.8 nm, respectively. By utilizing the DDRD technique, UV filters could be determined in the above ranges at 237.8, 241.0, and 254.2 nm, respectively. With the MCR technique, the UV filters could be determined in the above ranges at 381.7, 383.2, and 355.6 nm, respectively. The PLS-2 technique successfully quantified the examined UV filters in the ranges of 0.5-9.3, 0.3-7.1, and 0.5-6.9 μg/mL, respectively. All the methods were validated according to the International Conference on Harmonization guidelines and successfully applied to determine the UV filters in pure form, laboratory-prepared mixtures, and a sunscreen formulation. The obtained results were statistically compared with reference and reported methods of analysis for OXY, OMC, and OCR, and there were no significant differences with respect to accuracy and precision of the adopted techniques.

Sensitive flow-injection spectrophotometric analysis of bromopride

NASA Astrophysics Data System (ADS)

Lima, Liliane Spazzapam; Weinert, Patrícia Los; Pezza, Leonardo; Pezza, Helena Redigolo

2014-12-01

A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax = 565 nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63 × 10-7 to 2.90 × 10-5 mol L-1, with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07 × 10-7 and 3.57 × 10-7 mol L-1, respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps.

Sensitive flow-injection spectrophotometric analysis of bromopride.

PubMed

Lima, Liliane Spazzapam; Los Weinert, Patrícia; Pezza, Leonardo; Pezza, Helena Redigolo

2014-12-10

A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax=565nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63×10(-7) to 2.90×10(-5)molL(-1), with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07×10(-7) and 3.57×10(-7)molL(-1), respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of an reliable analytical method for synergistic extractive spectrophotometric determination of cobalt(II) from alloys and nano composite samples by using chromogenic chelating ligand

NASA Astrophysics Data System (ADS)

Kamble, Ganesh S.; Ghare, Anita A.; Kolekar, Sanjay S.; Han, Sung H.; Anuse, Mansing A.

2011-12-01

A synergistic simple and selective spectrophotometric method was developed for the determination of cobalt(II) with 1-(2',4'-dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydropyrimidine-2-thiol [2',4'-dinitro APTPT] as a chromogenic reagent. The proposed method has been described on the basis of synergistic effective extraction of cobalt(II) in presence of pyridine at pH range 9.5-10.2, showed orange-red coloured ternary complex having molar ratio 1:2:2 (M:L:Py). The equilibrium time is 10 min for extraction of cobalt(III) from organic phase. The absorbance of coloured organic layer in chloroform is measured spectrophotometrically at 490 nm against reagent blank. The Beer's law was obeyed in the concentration range 2.5-15 μg mL -1 of cobalt(II) and optimum concentration range was 5-12.5 μg mL -1 of cobalt(II) and it was evaluated from Ringbom's plot. The molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT-pyridine complex in chloroform are 1.109 × 10 3 L mol -1 cm -1 and 0.053 μg cm -2, respectively while molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT complex in chloroform are 6.22 × 10 2 L mol -1 cm -1 and 0.096 μg cm -2, respectively. The composition of cobalt(II)-2',4'-dinitro APTPT-pyridine complex (1:2:2) was established by slope ratio method, mole ratio method and Job's method of continuous variation. The ternary complex was stable for more than 48 h. The interfering effects of various cations and anions were also studied, and use of suitable masking agents enhances the selectivity of the method. The method is successfully applied for the determination of cobalt(II) in binary, synthetic mixtures and real samples. A repetition of the method was checked by finding relative standard deviation (R.S.D.) for n = 5 which was 0.15%. The reliability of the method is confirmed by comparison of experimental results with atomic absorption spectrophotometer.

Comparative Study of Novel Ratio Spectra and Isoabsorptive Point Based Spectrophotometric Methods: Application on a Binary Mixture of Ascorbic Acid and Rutin.

PubMed

Darwish, Hany W; Bakheit, Ahmed H; Naguib, Ibrahim A

2016-01-01

This paper presents novel methods for spectrophotometric determination of ascorbic acid (AA) in presence of rutin (RU) (coformulated drug) in their combined pharmaceutical formulation. The seven methods are ratio difference (RD), isoabsorptive_RD (Iso_RD), amplitude summation (A_Sum), isoabsorptive point, first derivative of the ratio spectra ((1)DD), mean centering (MCN), and ratio subtraction (RS). On the other hand, RU was determined directly by measuring the absorbance at 358 nm in addition to the two novel Iso_RD and A_Sum methods. The work introduced in this paper aims to compare these different methods, showing the advantages for each and making a comparison of analysis results. The calibration curve is linear over the concentration range of 4-50 μg/mL for AA and RU. The results show the high performance of proposed methods for the analysis of the binary mixture. The optimum assay conditions were established and the proposed methods were successfully applied for the assay of the two drugs in laboratory prepared mixtures and combined pharmaceutical tablets with excellent recoveries. No interference was observed from common pharmaceutical additives.

Comparative Study of Novel Ratio Spectra and Isoabsorptive Point Based Spectrophotometric Methods: Application on a Binary Mixture of Ascorbic Acid and Rutin

PubMed Central

Darwish, Hany W.; Bakheit, Ahmed H.; Naguib, Ibrahim A.

2016-01-01

This paper presents novel methods for spectrophotometric determination of ascorbic acid (AA) in presence of rutin (RU) (coformulated drug) in their combined pharmaceutical formulation. The seven methods are ratio difference (RD), isoabsorptive_RD (Iso_RD), amplitude summation (A_Sum), isoabsorptive point, first derivative of the ratio spectra (1DD), mean centering (MCN), and ratio subtraction (RS). On the other hand, RU was determined directly by measuring the absorbance at 358 nm in addition to the two novel Iso_RD and A_Sum methods. The work introduced in this paper aims to compare these different methods, showing the advantages for each and making a comparison of analysis results. The calibration curve is linear over the concentration range of 4–50 μg/mL for AA and RU. The results show the high performance of proposed methods for the analysis of the binary mixture. The optimum assay conditions were established and the proposed methods were successfully applied for the assay of the two drugs in laboratory prepared mixtures and combined pharmaceutical tablets with excellent recoveries. No interference was observed from common pharmaceutical additives. PMID:26885440

The ultraviolet detection component based on Te-Cs image intensifier

NASA Astrophysics Data System (ADS)

Qian, Yunsheng; Zhou, Xiaoyu; Wu, Yujing; Wang, Yan; Xu, Hua

2017-05-01

Ultraviolet detection technology has been widely focused and adopted in the fields of ultraviolet warning and corona detection for its significant value and practical meaning. The component structure of ultraviolet ICMOS, imaging driving and the photon counting algorithm are studied in this paper. Firstly, the one-inch and wide dynamic range CMOS chip with the coupling optical fiber panel is coupled to the ultraviolet image intensifier. The photocathode material in ultraviolet image intensifier is Te-Cs, which contributes to the solar blind characteristic, and the dual micro-channel plates (MCP) structure ensures the sufficient gain to achieve the single photon counting. Then, in consideration of the ultraviolet detection demand, the drive circuit of the CMOS chip is designed and the corresponding program based on Verilog language is written. According to the characteristics of ultraviolet imaging, the histogram equalization method is applied to enhance the ultraviolet image and the connected components labeling way is utilized for the ultraviolet single photon counting. Moreover, one visible light video channel is reserved in the ultraviolet ICOMS camera, which can be used for the fusion of ultraviolet and visible images. Based upon the module, the ultraviolet optical lens and the deep cut-off solar blind filter are adopted to construct the ultraviolet detector. At last, the detection experiment of the single photon signal is carried out, and the test results are given and analyzed.

Determination of tramadol hydrochloride in ampoule dosage forms by using UV spectrophotometric and HPLC-DAD methods in methanol and water media.

PubMed

Küçük, Aysel; Kadioğlu, Yücel

2005-02-01

Two newly developed simple and sensitive methods for determination of tramadol hydrochloride in ampoule dosage forms were described and validated. Measurements for spectrophotometric method were performed using UV-Vis Spectrophotometer in ranges of 200-400 nm. The solutions of standard and the samples were prepared in methanol and water media and the UV absorption spectrums of tramadol were monitored with maximum absorptions at 275 and 271 nm for both mediums, respectively. The standard calibration curves of tramadol were constructed by plotting absorbance vs. concentration in the concentration range with the final dilution of 10-100 microg ml-1. Reversed phase chromatography for HPLC method was conducted using a Phenomenex Bondclone C18 column with an isocratic mobile phase consisting of 25% acetonitrile in 75% 0.01 M phosphate buffer (pH 3). The effluent was monitored on a DAD detector at 218 nm. Linear response (r>0.99) was observed over the range of 0.5-40 microg ml-1 for methanol and water and run on six different occasions. The methods were applied successfully to pharmaceutical ampoule forms, but also for comparison in two different solvent media. Besides, it was completely validated and proven to be rugged.

Comparative study of three modified numerical spectrophotometric methods: An application on pharmaceutical ternary mixture of aspirin, atorvastatin and clopedogrel

NASA Astrophysics Data System (ADS)

Issa, Mahmoud Mohamed; Nejem, R.'afat Mahmoud; Shanab, Alaa Abu; Hegazy, Nahed Diab; Stefan-van Staden, Raluca-Ioana

2014-07-01

Three novel numerical methods were developed for the spectrophotometric multi-component analysis of capsules and synthetic mixtures of aspirin, atorvastatin and clopedogrel without any chemical separation. The subtraction method is based on the relationship between the difference in absorbance at four wavelengths and corresponding concentration of analyte. In this method, the linear determination ranges were 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 0.5-30 μg mL-1 clopedogrel. In the quotient method, 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 1.0-30 μg mL-1 clopedogrel were determine from spectral data at the wavelength pairs that show the same ratio of absorbance for other two species. Standard addition method was used for resolving ternary mixture of 1.0-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 2.0-30 μg mL-1 clopedogrel. The proposed methods were validated. The reproducibility and repeatability were found satisfactory which evidence was by low values of relative standard deviation (<2%). Recovery was found to be in the range (99.6-100.8%). By adopting these methods, the time taken for analysis was reduced as these methods involve very limited steps. The developed methods were applied for simultaneous analysis of aspirin, atorvastatin and clopedogrel in capsule dosage forms and results were in good concordance with alternative liquid chromatography.

Preparation and Spectrophotometric Analysis of Hexaamminenickel(II) Chloride.

ERIC Educational Resources Information Center

Wieder, Grace M.

1986-01-01

Describes an experiment developed at Brooklyn College (New York) in which the preparation and ammonia analysis of an amminenickel(II) chloride is extended to include a spectrophotometric analysis for nickel. Discusses the materials needed and the procedure for the experiment which takes nine hours of laboratory work. (TW)

Ultraviolet laser beam monitor using radiation responsive crystals

DOEpatents

McCann, Michael P.; Chen, Chung H.

1988-01-01

An apparatus and method for monitoring an ultraviolet laser beam includes disposing in the path of an ultraviolet laser beam a substantially transparent crystal that will produce a color pattern in response to ultraviolet radiation. The crystal is exposed to the ultraviolet laser beam and a color pattern is produced within the crystal corresponding to the laser beam intensity distribution therein. The crystal is then exposed to visible light, and the color pattern is observed by means of the visible light to determine the characteristics of the laser beam that passed through crystal. In this manner, a perpendicular cross sectional intensity profile and a longitudinal intensity profile of the ultraviolet laser beam may be determined. The observation of the color pattern may be made with forward or back scattered light and may be made with the naked eye or with optical systems such as microscopes and television cameras.

Development of deep-ultraviolet metal vapor lasers

NASA Astrophysics Data System (ADS)

Sabotinov, Nikola V.

2004-06-01

Deep ultraviolet laser generation is of great interest in connection with both the development of new industrial technologies and applications in medicine, biology, chemistry, etc. The development of metal vapor UV lasers oscillating in the pulsed mode with high pulse repetition frequencies and producing high average output powers is of particular interest for microprocessing of polymers, photolithography and fluorescence applications. At present, metal vapor lasers generate deep-UV radiation on the base of two methods. The first method is non-linear conversion of powerful laser generation from the visible region into the deep ultraviolet region. The second method is direct UV laser action on ion and atomic transitions of different metals.

Spectrophotometric and spectrofluorimetric determination of indacaterol maleate in pure form and pharmaceutical preparations: application to content uniformity.

PubMed

El-Ashry, S M; El-Wasseef, D R; El-Sherbiny, D T; Salem, Y A

2015-09-01

Two simple, rapid, sensitive and precise spectrophotometric and spectrofluorimetric methods were developed for the determination of indacaterol maleate in bulk powder and capsules. Both methods were based on the direct measurement of the drug in methanol. In the spectrophotometric method (Method I) the absorbance was measured at 259 nm. The absorbance-concentration plot was rectilinear over the range 1.0-10.0 µg mL(-1) with a lower detection limit (LOD) of 0.078 µg mL(-1) and lower quantification limit (LOQ) of 0.238 µg mL(-1). Meanwhile in the spectrofluorimetric method (Method II) the native fluorescence was measured at 358 nm after excitation at 258 nm. The fluorescence-concentration plot was rectilinear over the range of 1.0-40.0 ng mL(-1) with an LOD of 0.075 ng mL(-1) and an LOQ of 0.226 ng mL(-1). The proposed methods were successfully applied to the determination of indacaterol maleate in capsules with average percent recoveries ± RSD% of 99.94 ± 0.96 for Method I and 99.97 ± 0.81 for Method II. In addition, the proposed methods were extended to a content uniformity test according to the United States Pharmacopoeia (USP) guidelines and were accurate, precise for the capsules studied with acceptance value 3.98 for Method I and 2.616 for Method II. Copyright © 2015 John Wiley & Sons, Ltd.

Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods

NASA Astrophysics Data System (ADS)

Al Okab, Riyad Ahmed

2013-02-01

Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml-1 and molar absorptivity 1.41 × 104 L mol-1 cm-1. All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

Spectrophotometric determination of ternary mixtures of thiamin, riboflavin and pyridoxal in pharmaceutical and human plasma by least-squares support vector machines.

PubMed

Niazi, Ali; Zolgharnein, Javad; Afiuni-Zadeh, Somaie

2007-11-01

Ternary mixtures of thiamin, riboflavin and pyridoxal have been simultaneously determined in synthetic and real samples by applications of spectrophotometric and least-squares support vector machines. The calibration graphs were linear in the ranges of 1.0 - 20.0, 1.0 - 10.0 and 1.0 - 20.0 microg ml(-1) with detection limits of 0.6, 0.5 and 0.7 microg ml(-1) for thiamin, riboflavin and pyridoxal, respectively. The experimental calibration matrix was designed with 21 mixtures of these chemicals. The concentrations were varied between calibration graph concentrations of vitamins. The simultaneous determination of these vitamin mixtures by using spectrophotometric methods is a difficult problem, due to spectral interferences. The partial least squares (PLS) modeling and least-squares support vector machines were used for the multivariate calibration of the spectrophotometric data. An excellent model was built using LS-SVM, with low prediction errors and superior performance in relation to PLS. The root mean square errors of prediction (RMSEP) for thiamin, riboflavin and pyridoxal with PLS and LS-SVM were 0.6926, 0.3755, 0.4322 and 0.0421, 0.0318, 0.0457, respectively. The proposed method was satisfactorily applied to the rapid simultaneous determination of thiamin, riboflavin and pyridoxal in commercial pharmaceutical preparations and human plasma samples.

Kinetic Spectrophotometric Determination of Biotin in Pharmaceutical Preparations

PubMed Central

Walash, M. I.; Rizk, M.; Sheribah, Z. A.; Salim, M. M.

2008-01-01

A simple accurate kinetic spectrophotometric method was developed for the determination of biotin in pure form and pharmaceutical preparations. The proposed method is based on a catalytic acceleration of biotin on the reaction between sodium azide and tri-iodide in an aqueous solution. Concentration range of 4-16 μg/mL for biotin was determined by measuring the decrease in the absorbance of tri-iodide at 348 nm by a fixed time method. The decrease in absorbance after 14 min from the initiation of the reaction was markedly correlated to the concentration with correlation coefficient of 0.9999. The detection limit (LOD) of biotin was 0.18 μg/mL while quantitation limit (LOQ) was 0.54 μg/mL. The percentage recovery of the spiked samples was 100.08 ± 0.761. The proposed procedure was successfully applied for the determination of biotin in its pharmaceutical preparations with mean recoveries of 101.17 ± 2.05 and 97.87 ± 1.50 for biotin ampoules and capsules, respectively. The results obtained were in good agreement with those obtained using official method. PMID:23675096

In-situ spectrophotometric probe

DOEpatents

Prather, W.S.

1992-12-15

A spectrophotometric probe is described for in situ absorption spectra measurements comprising a first optical fiber carrying light from a remote light source, a second optical fiber carrying light to a remote spectrophotometer, the proximal ends of the first and second optical fibers parallel and co-terminal, a planoconvex lens to collimate light from the first optical fiber, a reflecting grid positioned a short distance from the lens to reflect the collimated light back to the lens for focusing on the second optical fiber. The lens is positioned with the convex side toward the optical fibers. A substrate for absorbing analyte or an analyte and reagent mixture may be positioned between the lens and the reflecting grid. 5 figs.

In-situ spectrophotometric probe

DOEpatents

Prather, William S.

1992-01-01

A spectrophotometric probe for in situ absorption spectra measurements comprising a first optical fiber carrying light from a remote light source, a second optical fiber carrying light to a remote spectrophotometer, the proximal ends of the first and second optical fibers parallel and coterminal, a planoconvex lens to collimate light from the first optical fiber, a reflecting grid positioned a short distance from the lens to reflect the collimated light back to the lens for focussing on the second optical fiber. The lens is positioned with the convex side toward the optical fibers. A substrate for absorbing analyte or an analyte and reagent mixture may be positioned between the lens and the reflecting grid.

A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection.

PubMed

Riad, Safaa M; El-Rahman, Mohamed K Abd; Fawaz, Esraa M; Shehata, Mostafa A

2015-06-15

Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 μg/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed. Copyright © 2015 Elsevier B.V. All rights reserved.

A simple spectrophotometric determination of meptyldinocap by its hydrolysis.

PubMed

Kurup, Sunita; Pillai, Ajai Kumar

2013-01-01

A simple spectrophotometric method is proposed for the determination of meptyldinocap (2,4-dinitro-6-octylphenyl crotonate). The method is based on the hydrolysis of meptyldinocap by hydroxylamine solution in alkaline medium to give 2,4-dinitro-6-octylphenol (2,4-DNOP), having maximum absorption at 380 nm. The reaction is found to be instantaneous in presence of ethanol. Beer's law is valid over the concentration range of 1.2-13 microg mL(-1) with molar absorptivity and Sandell's sensitivity of 3.22 x 10(6) L mol(-1) cm(-1) and 0.0001 microg cm(-2) respectively. The limit of detection and quantification were 0.0892 and 0.2703 microg mL(-1), respectively. The tolerance limits of interfering ions are discussed. All variables were studied in order to optimize the reaction conditions. The validity of the method was checked by its simultaneous determination in fruits and water samples and the results were statistically compared with those of a reference method by applying the Student's t-test and F-test.

Psoralen-ultraviolet A treatment with Psoralen-ultraviolet B therapy in the treatment of psoriasis.

PubMed

Ahmed Asim, Sadaf; Ahmed, Sitwat; Us-Sehar, Najam

2013-05-01

To compare the conventional psoralen-ultraviolet A treatment with psoralen-ultraviolet B therapy in the treatment of psoriasis. We studied 50 patients of plaque type psoriasis who were selected to receive either conventional psoralen-ultraviolet A or psoralen-ultraviolet B treatment. There was no significant difference between the two treatment groups in the number of patients whose skin cleared of psoriasis or the number of exposures required for clearance. Profile of side effects and disease status was also similar after three months of follow up. Psoralen-ultraviolet B treatment is as effective as conventional psoralen-ultraviolet A in the treatment of psoriasis. Further long term studies are needed to assess the safety of psoralen-ultraviolet B.

Development and validation of simple spectrophotometric and chemometric methods for simultaneous determination of empagliflozin and metformin: Applied to recently approved pharmaceutical formulation

NASA Astrophysics Data System (ADS)

Ayoub, Bassam M.

2016-11-01

New univariate spectrophotometric method and multivariate chemometric approach were developed and compared for simultaneous determination of empagliflozin and metformin manipulating their zero order absorption spectra with application on their pharmaceutical preparation. Sample enrichment technique was used to increase concentration of empagliflozin after extraction from tablets to allow its simultaneous determination with metformin without prior separation. Validation parameters according to ICH guidelines were satisfactory over the concentration range of 2-12 μg mL- 1 for both drugs using simultaneous equation with LOD values equal to 0.20 μg mL- 1 and 0.19 μg mL- 1, LOQ values equal to 0.59 μg mL- 1 and 0.58 μg mL- 1 for empagliflozin and metformin, respectively. While the optimum results for the chemometric approach using partial least squares method (PLS-2) were obtained using concentration range of 2-10 μg mL- 1. The optimized validated methods are suitable for quality control laboratories enable fast and economic determination of the recently approved pharmaceutical combination Synjardy® tablets.

Spectrophotometric determination of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid in pure form and in pharmaceuticals

NASA Astrophysics Data System (ADS)

Bazel, Yaroslav; Hunka, Iryna; Kormosh, Zholt; Andruch, Vasil

2009-12-01

A new sensitive and selective spectrophotometric method has been developed for the determination of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid in pharmaceuticals in the presence of nicotinic acid. The method is based on the reaction of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid with 1,3,3-trimethyl-5-phenyl-2-[3-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-propenyl]-3 H-indolium chloride (PIC) followed by the extraction of the formed ion associate into toluene and spectrophotometric detection at 581 nm. Appropriate experimental conditions were found to be pH 7.8-9.8 and 3.6 × 10 -4 mol L -1 of PIC. The molar absorptivity is 5.0 × 10 -4 L mol -1 cm -1. The absorbance obeys Beer's law in the range 0.61-12.60 μg mL -1 of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid, and the detection limit calculated from a blank test was 0.20 μg mL -1.

Spectrophotometric determination of fluorine in silicate rocks

USGS Publications Warehouse

Peck, L.C.; Smith, V.C.

1964-01-01

The rock powder is sintered with a sodium carbonate flux containing zinc oxide and magnesium carbonate, the sinter-cake leached with water and the resulting solution filtered. Fluorine is separated from the acidified filtrate by steam distillation and determined spectrophotometrically by means of a zirconium-SPADNS reagent. If a multiple-unit distillation apparatus is used, 12 determinations can be completed per man-day. ?? 1964.

Spectrophotometric Titration of a Mixture of Calcium and Magnesium.

ERIC Educational Resources Information Center

Fulton, Robert; And Others

1986-01-01

Describes a spectrophotometric titration experiment which uses a manual titration spectrophotometer and manually operated buret, rather than special instrumentation. Identifies the equipment, materials, and procedures needed for the completion of the experiment. Recommends the use of this experiment in introductory quantitative analysis…

Comparison of methods for measuring cholinesterase inhibition by carbamates

PubMed Central

Wilhelm, K.; Vandekar, M.; Reiner, E.

1973-01-01

The Acholest and tintometric methods are used widely for measuring blood cholinesterase activity after exposure to organophosphorus compounds. However, if applied for measuring blood cholinesterase activity in persons exposed to carbamates, the accuracy of the methods requires verification since carbamylated cholinesterases are unstable. The spectrophotometric method was used as a reference method and the two field methods were employed under controlled conditions. Human blood cholinesterases were inhibited in vitro by four methylcarbamates that are used as insecticides. When plasma cholinesterase activity was measured by the Acholest and spectrophotometric methods, no difference was found. The enzyme activity in whole blood determined by the tintometric method was ≤ 11% higher than when the same sample was measured by the spectrophotometric method. PMID:4541147

Yonsei Evolutionary Population Synthesis (YEPS). II. Spectro-photometric Evolution of Helium-enhanced Stellar Populations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chung, Chul; Yoon, Suk-Jin; Lee, Young-Wook, E-mail: chulchung@yonsei.ac.kr, E-mail: sjyoon0691@yonsei.ac.kr

The discovery of multiple stellar populations in Milky Way globular clusters (GCs) has stimulated various follow-up studies on helium-enhanced stellar populations. Here we present the evolutionary population synthesis models for the spectro-photometric evolution of simple stellar populations (SSPs) with varying initial helium abundance ( Y {sub ini}). We show that Y {sub ini} brings about dramatic changes in spectro-photometric properties of SSPs. Like the normal-helium SSPs, the integrated spectro-photometric evolution of helium-enhanced SSPs is also dependent on metallicity and age for a given Y {sub ini}. We discuss the implications and prospects for the helium-enhanced populations in relation to themore » second-generation populations found in the Milky Way GCs. All of the models are available at http://web.yonsei.ac.kr/cosmic/data/YEPS.htm.« less

Simultaneous determination of mebeverine hydrochloride and chlordiazepoxide in their binary mixture using novel univariate spectrophotometric methods via different manipulation pathways.

PubMed

Lotfy, Hayam M; Fayez, Yasmin M; Michael, Adel M; Nessim, Christine K

2016-02-15

Smart, sensitive, simple and accurate spectrophotometric methods were developed and validated for the quantitative determination of a binary mixture of mebeverine hydrochloride (MVH) and chlordiazepoxide (CDZ) without prior separation steps via different manipulating pathways. These pathways were applied either on zero order absorption spectra namely, absorbance subtraction (AS) or based on the recovered zero order absorption spectra via a decoding technique namely, derivative transformation (DT) or via ratio spectra namely, ratio subtraction (RS) coupled with extended ratio subtraction (EXRS), spectrum subtraction (SS), constant multiplication (CM) and constant value (CV) methods. The manipulation steps applied on the ratio spectra are namely, ratio difference (RD) and amplitude modulation (AM) methods or applying a derivative to these ratio spectra namely, derivative ratio (DD(1)) or second derivative (D(2)). Finally, the pathway based on the ratio spectra of derivative spectra is namely, derivative subtraction (DS). The specificity of the developed methods was investigated by analyzing the laboratory mixtures and was successfully applied for their combined dosage form. The proposed methods were validated according to ICH guidelines. These methods exhibited linearity in the range of 2-28μg/mL for mebeverine hydrochloride and 1-12μg/mL for chlordiazepoxide. The obtained results were statistically compared with those of the official methods using Student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Psoralen-ultraviolet A treatment with Psoralen-ultraviolet B therapy in the treatment of psoriasis

PubMed Central

Ahmed Asim, Sadaf; Ahmed, Sitwat; us-Sehar, Najam

2013-01-01

Objective: To compare the conventional psoralen-ultraviolet A treatment with psoralen-ultraviolet B therapy in the treatment of psoriasis. Methodology: We studied 50 patients of plaque type psoriasis who were selected to receive either conventional psoralen-ultraviolet A or psoralen-ultraviolet B treatment. Results: There was no significant difference between the two treatment groups in the number of patients whose skin cleared of psoriasis or the number of exposures required for clearance. Profile of side effects and disease status was also similar after three months of follow up. Conclusion: Psoralen-ultraviolet B treatment is as effective as conventional psoralen-ultraviolet A in the treatment of psoriasis. Further long term studies are needed to assess the safety of psoralen-ultraviolet B. PMID:24353623

Simple, sensitive, selective and validated spectrophotometric methods for the estimation of a biomarker trigonelline from polyherbal gels

NASA Astrophysics Data System (ADS)

Chopra, Shruti; Motwani, Sanjay K.; Ahmad, Farhan J.; Khar, Roop K.

2007-11-01

Simple, accurate, reproducible, selective, sensitive and cost effective UV-spectrophotometric methods were developed and validated for the estimation of trigonelline in bulk and pharmaceutical formulations. Trigonelline was estimated at 265 nm in deionised water and at 264 nm in phosphate buffer (pH 4.5). Beer's law was obeyed in the concentration ranges of 1-20 μg mL -1 ( r2 = 0.9999) in deionised water and 1-24 μg mL -1 ( r2 = 0.9999) in the phosphate buffer medium. The apparent molar absorptivity and Sandell's sensitivity coefficient were found to be 4.04 × 10 3 L mol -1 cm -1 and 0.0422 μg cm -2/0.001A in deionised water; and 3.05 × 10 3 L mol -1 cm -1 and 0.0567 μg cm -2/0.001A in phosphate buffer media, respectively. These methods were tested and validated for various parameters according to ICH guidelines. The detection and quantitation limits were found to be 0.12 and 0.37 μg mL -1 in deionised water and 0.13 and 0.40 μg mL -1 in phosphate buffer medium, respectively. The proposed methods were successfully applied for the determination of trigonelline in pharmaceutical formulations (vaginal tablets and bioadhesive vaginal gels). The results demonstrated that the procedure is accurate, precise, specific and reproducible (percent relative standard deviation <2%), while being simple and less time consuming and hence can be suitably applied for the estimation of trigonelline in different dosage forms and dissolution studies.

Micellar modified spectrophotometric determination of nitrobenzenes based upon reduction with tin(II), diazotisation and coupling with the Bratton-Marshall reagent.

PubMed

Escrig-Tena, I; Alvarez Rodríguez, L; Esteve-Romero, J; García-Alvarez-Coque, M C

1998-09-01

Nitrobenzenes, such as the antibiotic chloramphenicol, the vasodilator nicardipine, and the herbicides dinitramin, dinobuton, fenitrothion, methylparathion, oxyfluorfen, parathion, pendimethalin, quintozene, and trifluralin, were determined by using a spectrophotometric method in the visible region (540 nm). The method was based on the reduction of the nitrobenzenes to arylamines with tin(II) chloride, diazotisation of the arylamines and coupling of the diazonium ions with the Bratton-Marshall reagent. The two latter reactions were performed in a micellar medium of sodium dodecyl sulphate. The linear calibration range was 2x10(-6) to 7x10(-5) M (r>0.999), with limits of detection in the 10(-7) M level, which is 2-6 fold lower with respect to the corresponding spectrophotometric procedure in non-micellar medium. The procedure was applied to the analysis of the compounds in commercial preparations (pharmaceuticals and herbicide formulations) and in water samples, with good recoveries.

Precision Spectrophotometric Calibration System for Dark Energy Instruments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schubnell, Michael S.

2015-06-30

For this research we build a precision calibration system and carried out measurements to demonstrate the precision that can be achieved with a high precision spectrometric calibration system. It was shown that the system is capable of providing a complete spectrophotometric calibration at the sub-pixel level. The calibration system uses a fast, high precision monochromator that can quickly and efficiently scan over an instrument’s entire spectral range with a spectral line width of less than 0.01 nm corresponding to a fraction of a pixel on the CCD. The system was extensively evaluated in the laboratory. Our research showed that amore » complete spectrophotometric calibration standard for spectroscopic survey instruments such as DESI is possible. The monochromator precision and repeatability to a small fraction of the DESI spectrograph LSF was demonstrated with re-initialization on every scan and thermal drift compensation by locking to multiple external line sources. A projector system that mimics telescope aperture for point source at infinity was demonstrated.« less

Spectrophotometric determination of ofloxacin in pharmaceuticals by redox reaction

NASA Astrophysics Data System (ADS)

Ramesh, P. J.; Basavaiah, K.; Rajendraprasad, N.; Devi, O. Zenita; Vinay, K. B.

2011-07-01

Two simple spectrophotometric methods have been developed to analyze ofloxacin (OFX) in pharmaceuticals. The methods are based on the oxidation of OFX by a measured excess of cerium(IV) sulfate in H2SO4 medium. This was followed by the determination of the unreacted oxidant by reacting it with either p-toluidine ( p-TD) and measuring the absorbance at 525 nm (method A) or o-dianisidine ( o-DA) and measuring the absorbance at 470 nm (method B). In both methods, the amount of cerium(IV) sulfate reacted corresponds to the amount of OFX. Calibration graphs were linear over the ranges of 0-120 and 0-4 g/ml OFX for methods A and B, respectively. The calculated molar absorptivity (2.34ṡ103 and 5.99ṡ104), Sandell sensitivity, and limit of quantification for the methods are reported. The intra-day precision (%RSD) and accuracy (%RE) were < 8.0 and ≤ 4.0%, respectively, and the inter-day RSD and RE values were within 5 and 4.0%, respectively. The applicability of the methods was demonstrated by determining OFX in tablets with an accuracy (%RE) of < 3% and precision (%RSD) of ≤2.65%. The accuracy of the methods was further ascertained by recovery experiments via a standard-addition procedure.

Simplified 2,4-dinitrophenylhydrazine spectrophotometric assay for quantification of carbonyls in oxidized proteins.

PubMed

Mesquita, Cristina S; Oliveira, Raquel; Bento, Fátima; Geraldo, Dulce; Rodrigues, João V; Marcos, João C

2014-08-01

This work proposes a modification of the 2,4-dinitrophenylhydrazine (DNPH) spectrophotometric assay commonly used to evaluate the concentration of carbonyl groups in oxidized proteins. In this approach NaOH is added to the protein solution after the addition of DNPH, shifting the maximum absorbance wavelength of the derivatized protein from 370 to 450nm. This reduces the interference of DNPH and allows the direct quantification in the sample solution without the need for the precipitation, washing, and resuspension steps that are carried out in the traditional DNPH method. The two methods were compared under various conditions and are statistically equivalent. Copyright © 2014 Elsevier Inc. All rights reserved.

An estimation methode for measurement of ultraviolet radiation during nondestructive testing

NASA Astrophysics Data System (ADS)

Hosseinipanah, M.; Movafeghi, A.; Farvadin, D.

2018-04-01

Dye penetrant testing and magnetic particle testing are among conventional NDT methods. For increased sensitivity, fluorescence dyes and particles can be used with ultraviolet (black) lights. UV flaw detection lights have different spectra. With the help of photo-filters, the output lights are transferred to UV-A and visible zones. UV-A light can be harmful to human eyes in some conditions. In this research, UV intensity and spectrum were obtained by a Radio-spectrometer for two different UV flaw detector lighting systems. According to the standards such as ASTM E709, UV intensity must be at least 10 W/m2 at a distance of 30 cm. Based on our measurements; these features not achieved in some lamps. On the other hand, intensity and effective intensity of UV lights must be below the some limits for prevention of unprotected eye damage. NDT centers are usually using some type of UV measuring devices. A method for the estimation of effective intensity of UV light has been proposed in this research.

Simultaneous estimation of ramipril, acetylsalicylic acid and atorvastatin calcium by chemometrics assisted UV-spectrophotometric method in capsules.

PubMed

Sankar, A S Kamatchi; Vetrichelvan, Thangarasu; Venkappaya, Devashya

2011-09-01

In the present work, three different spectrophotometric methods for simultaneous estimation of ramipril, aspirin and atorvastatin calcium in raw materials and in formulations are described. Overlapped data was quantitatively resolved by using chemometric methods, viz. inverse least squares (ILS), principal component regression (PCR) and partial least squares (PLS). Calibrations were constructed using the absorption data matrix corresponding to the concentration data matrix. The linearity range was found to be 1-5, 10-50 and 2-10 μg mL-1 for ramipril, aspirin and atorvastatin calcium, respectively. The absorbance matrix was obtained by measuring the zero-order absorbance in the wavelength range between 210 and 320 nm. A training set design of the concentration data corresponding to the ramipril, aspirin and atorvastatin calcium mixtures was organized statistically to maximize the information content from the spectra and to minimize the error of multivariate calibrations. By applying the respective algorithms for PLS 1, PCR and ILS to the measured spectra of the calibration set, a suitable model was obtained. This model was selected on the basis of RMSECV and RMSEP values. The same was applied to the prediction set and capsule formulation. Mean recoveries of the commercial formulation set together with the figures of merit (calibration sensitivity, selectivity, limit of detection, limit of quantification and analytical sensitivity) were estimated. Validity of the proposed approaches was successfully assessed for analyses of drugs in the various prepared physical mixtures and formulations.

Novel Spectrophotometric Method for the Quantitation of Urinary Xanthurenic Acid and Its Application in Identifying Individuals with Hyperhomocysteinemia Associated with Vitamin B6 Deficiency

PubMed Central

Chen, Chi-Fen; Liu, Tsan-Zon; Lan, Wu-Hsiang; Wu, Li-An; Tsai, Chin-Hung; Chiou, Jeng-Fong; Tsai, Li-Yu

2013-01-01

A novel spectrophotometric method for the quantification of urinary xanthurenic acid (XA) is described. The direct acid ferric reduction (DAFR) procedure was used to quantify XA after it was purified by a solid-phase extraction column. The linearity of proposed method extends from 2.5 to 100.0 mg/L. The method is precise, yielding day-to-day CVs for two pooled controls of 3.5% and 4.6%, respectively. Correlation studies with an established HPLC method and a fluorometric procedure showed correlation coefficients of 0.98 and 0.98, respectively. Interference from various urinary metabolites was insignificant. In a small-scale screening of elderly conducted at Penghu county in Taiwan (n = 80), we were able to identify a group of twenty individuals having hyperhomocysteinemia (>15 μmole/L). Three of them were found to be positive for XA as analyzed by the proposed method, which correlated excellently with the results of the activation coefficient method for RBC's AST/B6 functional test. These data confirm the usefulness of the proposed method for identifying urinary XA as an indicator of vitamin B6 deficiency-associated hyperhomocysteinemic condition. PMID:24151616

Discuss the testing problems of ultraviolet irradiance meters

NASA Astrophysics Data System (ADS)

Ye, Jun'an; Lin, Fangsheng

2014-09-01

Ultraviolet irradiance meters are widely used in many areas such as medical treatment, epidemic prevention, energy conservation and environment protection, computers, manufacture, electronics, ageing of material and photo-electric effect, for testing ultraviolet irradiance intensity. So the accuracy of value directly affects the sterile control in hospital, treatment, the prevention level of CDC and the control accuracy of curing and aging in manufacturing industry etc. Because the display of ultraviolet irradiance meters is easy to change, in order to ensure the accuracy, it needs to be recalibrated after being used period of time. By the comparison with the standard ultraviolet irradiance meters, which are traceable to national benchmarks, we can acquire the correction factor to ensure that the instruments working under accurate status and giving the accurate measured data. This leads to an important question: what kind of testing device is more accurate and reliable? This article introduces the testing method and problems of the current testing device for ultraviolet irradiance meters. In order to solve these problems, we have developed a new three-dimensional automatic testing device. We introduce structure and working principle of this system and compare the advantages and disadvantages of two devices. In addition, we analyses the errors in the testing of ultraviolet irradiance meters.

Synthesis and investigation of antimicrobial activity and spectrophotometric and dyeing properties of some novel azo disperse dyes based on naphthalimides.

PubMed

Shaki, Hanieh; Gharanjig, Kamaladin; Khosravi, Alireza

2015-01-01

A series of novel disperse dyes containing azo group were synthesized through a diazotization and coupling process. The 4-amino-N-2-aminomethylpyridine-1,8-naphthalimide was diazotized by nitrosylsulphuric acid and coupled with various aromatic amines such as N,N-diethylaniline, N,N-dihydroxyethylaniline, 8-hydroxyquinoline, and 2-methylindole. Chemical structures of the synthesized dyes were characterized by Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), proton nuclear magnetic resonance ((1) H NMR), carbon nuclear magnetic resonance ((13) C NMR), elemental analysis, and ultraviolet-visible (UV-visible) spectroscopy. The spectrophotometric data of all dyes were evaluated in various solvents with different polarity. Eventually, the dyes were applied on polyamide fabrics in order to investigate their dyeing properties. The fastness properties of the dyed fabrics such as wash, light, and rubbing fastness degrees were measured by standard methods. Moreover, the color gamut of the synthesized dyes was measured on polyamide fabrics. Results indicated that some of the synthesized dyes were able to dye polyamide fabrics with deep shades. They had very good wash and rubbing fastness degrees and moderate-to-good light fastness on polyamide fabrics. The antibacterial and antifungal activities of the synthesized dyes were evaluated in soluble state and on the dyed fabrics. The results indicated that dye 2 containing N,N-dihydroxyethylaniline as coupler had the highest activity against all the bacteria and fungi used. © 2015 American Institute of Chemical Engineers.

Sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzene diazonium ion.

PubMed

Aderibigbe, Segun A; Adegoke, Olajire A; Idowu, Olakunle S; Olaleye, Sefiu O

2012-01-01

The study is a description of a sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzenediazonium ion (CDNBD). Spot test and thin layer chromatography revealed the formation of a new compound distinct from CDNBD and aceclofenac. Optimization studies established a reaction time of 5 min at 30 degrees C after vortex mixing the drug/CDNBD for 10 s. An absorption maximum of 430 nm was selected as analytical wavelength. A linear response was observed over 1.2-4.8 μg/mL of aceclofenac with a correlation coefficient of 0.9983 and the drug combined with CDNBD at stoichiometric ratio of 2 : 1. The method has a limit of detection of 0.403 μg/mL, limit of quantitation of 1.22 μg/mL and is reproducible over a three day assessment. The method gave Sandell's sensitivity of 3.279 ng/cm2. Intra- and inter-day accuracies (in terms of errors) were less than 6% while precisions were of the order of 0.03-1.89% (RSD). The developed spectrophotometric method is of equivalent accuracy (p > 0.05) with British Pharmacopoeia, 2010 potentiometric method. It has the advantages of speed, simplicity, sensitivity and more affordable instrumentation and could found application as a rapid and sensitive analytical method of aceclofenac. It is the first described method by azo dye derivatization for the analysis of aceclofenac in bulk samples and dosage forms.

Spectrophotometric determination of irrigant extrusion using passive ultrasonic irrigation, EndoActivator, or syringe irrigation.

PubMed

Rodríguez-Figueroa, Carolina; McClanahan, Scott B; Bowles, Walter R

2014-10-01

Sodium hypochlorite (NaOCl) irrigation is critical to endodontic success, and several new methods have been developed to improve irrigation efficacy (eg, passive ultrasonic irrigation [PUI] and EndoActivator [EA]). Using a novel spectrophotometric method, this study evaluated NaOCl irrigant extrusion during canal irrigation. One hundred fourteen single-rooted extracted teeth were decoronated to leave 15 mm of the root length for each tooth. Cleaning and shaping of the teeth were completed using standardized hand and rotary instrumentation to an apical file size #40/0.04 taper. Roots were sealed (not apex), and 54 straight roots (n = 18/group) and 60 curved roots (>20° curvature, n = 20/group) were included. Teeth were irrigated with 5.25% NaOCl by 1 of 3 methods: passive irrigation with needle, PUI, or EA irrigation. Extrusion of NaOCl was evaluated using a pH indicator and a spectrophotometer. Standard curves were prepared with known amounts of irrigant to quantify amounts in unknown samples. Irrigant extrusion was minimal with all methods, with most teeth showing no NaOCl extrusion in straight or curved roots. Minor NaOCl extrusion (1-3 μL) in straight roots or curved roots occurred in 10%-11% of teeth in all 3 irrigant methods. Two teeth in both the syringe irrigation and the EA group extruded 3-10 μL of NaOCl. The spectrophotometric method used in this study proved to be very sensitive while providing quantification of the irrigant levels extruded. Using the PUI or EA tip to within 1 mm of the working length appears to be fairly safe, but apical anatomy can vary in teeth to allow extrusion of irrigant. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Application of inorganic oxidants to the spectrophotometric determination of ribavirin in bulk and capsules.

PubMed

Darwish, Ibrahim A; Khedr, Alaa S; Askal, Hassan F; Mohamed, Ramadan M

2006-01-01

Eight spectrophotometric methods for determination of ribavirin have been developed and validated. These methods were based on the oxidation of the drug by different inorganic oxidants: ceric ammonium sulfate, potassium permanganate, ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate. The oxidation reactions were performed in perchloric acid medium for ceric ammonium sulfate and in sulfuric acid medium for the other reagents. With ceric ammonium sulfate and potassium permanganate, the concentration of ribavirin in its samples was determined by measuring the decrease in the absorption intensity of the colored reagents at 315 and 525 nm, respectively. With the other reagents, the concentration of ribavirin was determined by measuring the intensity of the developed colored reaction products at the wavelengths of maximum absorbance: 675, 780, 595, 595, 475, and 475 nm for reactions with ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate, respectively. Different variables affecting the reaction conditions were carefully studied and optimized. Under the optimum conditions, linear relationships with good correlation coefficients (0.9984-0.9998) were found between the absorbance readings and the concentrations of ribavirin in the range of 4-1400 microg/mL. The molar absorptivities were correlated with the oxidation potential of the oxidants used. The precision of the methods were satisfactory; the values of relative standard deviation did not exceed 1.64%. The proposed methods were successfully applied to the analysis of ribavirin in pure drug material and capsules with good accuracy and precision; the recovery values were 99.2-101.2 +/- 0.48-1.30%. The results obtained using the proposed spectrophotometric methods were comparable with those obtained with the official method stated in the United States Pharmacopeia.

Validated selective spectrophotometric methods for the kinetic determination of desloratidine in tablets and in the presence of its parent drug.

PubMed

Derayea, S M Sayed

2014-11-01

Two novel selective validated methods have been developed for analysis of desloratidine (DSL) in its tablets formulation. Both were kinetic spectrophotometric methods, depend on the interaction of the secondary amino group in DSL with acetaldehyde to give N-vinylpiperidyl product. The formed N-vinylpiperidyl compound was reacted with 2,3,5,6-tetrachloro-1,4-benzoquinone (chloranil) to form colored N-vinylpiperidyl-substituted benzoquinone derivatives. The formed blue-colored derivative was measured at 672 nm. The reaction conditions were carefully studied and all factors were optimized. The molar ratio between the reactants was estimated and a suggested reaction mechanism was presented. The analysis was carried out using initial rate and fixed time (at 6 min) methods. The linear concentration ranges were 3-50 and 10 - 60 μg mL-1 with limits of detection of 3.2 and 2.2 μg mL-1 for the initial rate and fixed time methods, respectively. ICH guidelines were applied for analytical performance validation of the proposed methods. The presence of common excipients in the pharmaceutical formulation did not produce any significant interference, as well as from loratadine, which is the parent compound of DSL. Different commercially available tablets formulations containing were successfully analyzed, with, the percentage recovery ranging from 97.28-100.90 ± 0.7 2-1.41%. The obtained results were compared statistically with the reported method results. The proposed methods have similar accuracy and precision as the reported as indicated from the F- and t-test data.

Spectrophotometric and chemometric methods for determination of imipenem, ciprofloxacin hydrochloride, dexamethasone sodium phosphate, paracetamol and cilastatin sodium in human urine

NASA Astrophysics Data System (ADS)

El-Kosasy, A. M.; Abdel-Aziz, Omar; Magdy, N.; El Zahar, N. M.

2016-03-01

New accurate, sensitive and selective spectrophotometric and chemometric methods were developed and subsequently validated for determination of Imipenem (IMP), ciprofloxacin hydrochloride (CIPRO), dexamethasone sodium phosphate (DEX), paracetamol (PAR) and cilastatin sodium (CIL) in human urine. These methods include a new derivative ratio method, namely extended derivative ratio (EDR), principal component regression (PCR) and partial least-squares (PLS) methods. A novel EDR method was developed for the determination of these drugs, where each component in the mixture was determined by using a mixture of the other four components as divisor. Peak amplitudes were recorded at 293.0 nm, 284.0 nm, 276.0 nm, 257.0 nm and 221.0 nm within linear concentration ranges 3.00-45.00, 1.00-15.00, 4.00-40.00, 1.50-25.00 and 4.00-50.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively. PCR and PLS-2 models were established for simultaneous determination of the studied drugs in the range of 3.00-15.00, 1.00-13.00, 4.00-12.00, 1.50-9.50, and 4.00-12.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively, by using eighteen mixtures as calibration set and seven mixtures as validation set. The suggested methods were validated according to the International Conference of Harmonization (ICH) guidelines and the results revealed that they were accurate, precise and reproducible. The obtained results were statistically compared with those of the published methods and there was no significant difference.

Improved spectrophotometric cell for hydrothermal solutions

USGS Publications Warehouse

Susak, N.J.; Crerar, D.A.; Forseman, T.C.; Haas, J.L.

1981-01-01

A simple, inexpensive spectrophotometric cell was designed for use with aqueous solutions for which temperature is a maximum of 325??C and pressure, 28 MPa. The cell has an internal volume of 5 ml and a path length of 1.31 cm. Each furnace assembly is 120 mm in diameter ?? 150 mm high and will fit into most commercial spectrophotometers. Temperature is controlled by a standard set-point controller and a balancing circuit that is used to maintain the temperature of the sample and reference cell within 1??C of each other at any temperature.

A simple spectrophotometric method for the determination of arsenic in industrial and environmental samples using 2,4-Dihydroxy benzophenone-2-amino thiophenol.

PubMed

Deepa, K; Lingappa, Y

2014-04-24

2,4-Dihydroxy benzophenone-2-amino thiophenol (BPBT) has been proposed as new analytical reagent for the direct non-extractive spectrophotometric determination of arsenic. The reagent reacts with arsenic in acidic medium (pH=6.0, sodium acetate-acetic acid buffer) to form light greenish yellow colored 1:1 (M:L) complex. Maximum absorbance was obtained at 343 nm and remains constant for over 24 h. The molar absorptivity and Sandell's sensitivity of BPBT are found to be 6.01×10(4) L mol(-1)cm(-1) and 0.0016 μg cm(-2) respectively. The system obeys Beer's law in the range of 0.125-2.637 μg/ml of As (III). Since BPBT method is more sensitive, it was applied for the determination of arsenic in some environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Ultraviolet-C Irradiation: A Novel Pasteurization Method for Donor Human Milk

PubMed Central

Christen, Lukas; Lai, Ching Tat; Hartmann, Ben; Hartmann, Peter E.; Geddes, Donna T.

2013-01-01

Background Holder pasteurization (milk held at 62.5°C for 30 minutes) is the standard treatment method for donor human milk. Although this method of pasteurization is able to inactivate most bacteria, it also inactivates important bioactive components. Therefore, the objective of this study was to investigate ultraviolet irradiation as an alternative treatment method for donor human milk. Methods Human milk samples were inoculated with five species of bacteria and then UV-C irradiated. Untreated and treated samples were analysed for bacterial content, bile salt stimulated lipase (BSSL) activity, alkaline phosphatase (ALP) activity, and fatty acid profile. Results All five species of bacteria reacted similarly to UV-C irradiation, with higher dosages being required with increasing concentrations of total solids in the human milk sample. The decimal reduction dosage was 289±17 and 945±164 J/l for total solids of 107 and 146 g/l, respectively. No significant changes in the fatty acid profile, BSSL activity or ALP activity were observed up to the dosage required for a 5-log10 reduction of the five species of bacteria. Conclusion UV-C irradiation is capable of reducing vegetative bacteria in human milk to the requirements of milk bank guidelines with no loss of BSSL and ALP activity and no change of FA. PMID:23840820

New Spectrophotometric Assay of Pyrantel Pamoate in Pharmaceuticals and Spiked Human Urine Using Three Complexing Agents

NASA Astrophysics Data System (ADS)

Swamy, N.; Prashanth, K. N.; Basavaiah, K.

2015-07-01

Three simple, rapid, inexpensive, and highly sensitive spectrophotometric methods are described for the quantifi cation of pyrantel pamoate (PYP) in pure drug and formulations. The methods are based on the molecular charge-transfer (CT) complexation reaction involving pyrantel base (PYL) as n-donor and iodine as σ-acceptor (I 2 , method A), and 2,4-dinitrophenol (DNP, method B) or picric acid (PA, method C) as π-acceptors. Spectrophotometrically, the CT complexes showed absorption maxima at 380, 420, and 430 nm, for methods A, B, and C, respectively. Under optimum conditions, Beer's law was obeyed over the concentration ranges 0.12-2.9, 0.12-3.75, and 0.12-2.9 μg/ml for methods A, B, and C, respectively. The apparent molar absorptivity of the CT complexes at the respective λmax are calculated to be 2.63 × 10 5 , 6.91 × 10 4 , and 1.73 × 10 5 l/mol· cm respectively and the corresponding Sandell sensitivity values are 0.0009, 0.003, and 0.0012. The limits of detection (LOD) and quantification (LOQ) are calculated to be (0.02 and 0.07), (0.05 and 0.15), and (0.02 and 0.07) μg/ml with methods A, B, and C, respectively. The intra-day and inter-day accuracy expressed as %RE and precision expressed as %RSD are less than 3%. The methods have been applied to the determination of PYP in tablets, suspensions, and spiked human urine. Parallel assay by a reference method and statistical analysis of the results obtained show no significant difference between the proposed methods and the reference method with respect to accuracy and precision, as evident from the Student's t and variation ratio tests. The accuracy of the methods has been further ascertained by recovery tests via the standard addition technique.

Ultraviolet-C Irradiation: A Novel Pasteurization Method for Donor Human Milk.

PubMed

Christen, Lukas; Lai, Ching Tat; Hartmann, Ben; Hartmann, Peter E; Geddes, Donna T

2013-01-01

Holder pasteurization (milk held at 62.5°C for 30 minutes) is the standard treatment method for donor human milk. Although this method of pasteurization is able to inactivate most bacteria, it also inactivates important bioactive components. Therefore, the objective of this study was to investigate ultraviolet irradiation as an alternative treatment method for donor human milk. Human milk samples were inoculated with five species of bacteria and then UV-C irradiated. Untreated and treated samples were analysed for bacterial content, bile salt stimulated lipase (BSSL) activity, alkaline phosphatase (ALP) activity, and fatty acid profile. All five species of bacteria reacted similarly to UV-C irradiation, with higher dosages being required with increasing concentrations of total solids in the human milk sample. The decimal reduction dosage was 289±17 and 945±164 J/l for total solids of 107 and 146 g/l, respectively. No significant changes in the fatty acid profile, BSSL activity or ALP activity were observed up to the dosage required for a 5-log10 reduction of the five species of bacteria. UV-C irradiation is capable of reducing vegetative bacteria in human milk to the requirements of milk bank guidelines with no loss of BSSL and ALP activity and no change of FA.

Pyrocatechol violet in pharmaceutical analysis. Part I. A spectrophotometric method for the determination of some beta-lactam antibiotics in pure and in pharmaceutical dosage forms.

PubMed

Amin, A S

2001-03-01

A fairly sensitive, simple and rapid spectrophotometric method for the determination of some beta-lactam antibiotics, namely ampicillin (Amp), amoxycillin (Amox), 6-aminopenicillanic acid (6APA), cloxacillin (Clox), dicloxacillin (Diclox) and flucloxacillin sodium (Fluclox) in bulk samples and in pharmaceutical dosage forms is described. The proposed method involves the use of pyrocatechol violet as a chromogenic reagent. These drugs produce a reddish brown coloured ion pair with absorption maximum at 604, 641, 645, 604, 649 and 641 nm for Amp, Amox, 6APA, Clox, Diclox and Flucolx, respectively. The colours produced obey Beer's law and are suitable for the quantitative determination of the named compounds. The optimization of different experimental conditions is described. The molar ratio of the ion pairs was established and a proposal for the reaction pathway is given. The procedure described was applied successfully to determine the examined drugs in dosage forms and the results obtained were comparable to those obtained with the official methods.

Sustained prediction ability of net analyte preprocessing methods using reduced calibration sets. Theoretical and experimental study involving the spectrophotometric analysis of multicomponent mixtures.

PubMed

Goicoechea, H C; Olivieri, A C

2001-07-01

A newly developed multivariate method involving net analyte preprocessing (NAP) was tested using central composite calibration designs of progressively decreasing size regarding the multivariate simultaneous spectrophotometric determination of three active components (phenylephrine, diphenhydramine and naphazoline) and one excipient (methylparaben) in nasal solutions. Its performance was evaluated and compared with that of partial least-squares (PLS-1). Minimisation of the calibration predicted error sum of squares (PRESS) as a function of a moving spectral window helped to select appropriate working spectral ranges for both methods. The comparison of NAP and PLS results was carried out using two tests: (1) the elliptical joint confidence region for the slope and intercept of a predicted versus actual concentrations plot for a large validation set of samples and (2) the D-optimality criterion concerning the information content of the calibration data matrix. Extensive simulations and experimental validation showed that, unlike PLS, the NAP method is able to furnish highly satisfactory results when the calibration set is reduced from a full four-component central composite to a fractional central composite, as expected from the modelling requirements of net analyte based methods.

Spectrophotometric determination of bacitracin in bulk drug as dabsyl derivative in a range of visible light.

PubMed

Krzek, Jan; Piotrowska, Joanna

2011-01-01

A fast spectrophotometric method has been developed for bacitracin identification and determination after condensation reaction with dabsyl chloride. In addition, determination of dye stability of sulfonamide derivative and identification of the molar ratio of reagents was done at various time-points. The developed method has a good linearity with very broad spectrum, correlation coefficient of r = 0.9972, good precision (RSD = 1.54 +/- 0.11%), and recovery at three different levels of concentration was found between 98.33% and 103.47%. Usefulness of the method was demonstrated by positive results obtained during determination of bacitracin concentration in bulk drug.

VizieR Online Data Catalog: Spectrophotometric Standards near the Pole (Tereshchenko, 1994)

NASA Astrophysics Data System (ADS)

Tereshchenko, V. M.

1997-01-01

Absolute energy distributions for 13 circumpolar (δ>+85deg) stars forming a spectrophotometric version of the North Polar Spectrophotometric Sequence (NPSS) are presented. A-type stars of 5-9mag brightness were studied in the range 3100 to 7750A with resolution of 50A. Observations were made with 0.5-m and 1-m telescopes using Seya-Namioka spectrometers. The relative rms error of results in the region 4000-7000A is 2 to 3%, while at the ends of the studied range it is 3-5%. The primary standard was the circumpolar star HD 221525 (V=5.58, A7IV), and its spectral energy distribution had been determined earlier. (1 data file).

A spectrophotometric biochemical oxygen demand determination method using 2,6-dichlorophenolindophenol as the redox color indicator and the eukaryote Saccharomyces cerevisiae.