scholarly journals Spectrophotometric and Conductometric Determination of Clomiphene Citrate and Nefazodone HCl

2008 ◽  
Vol 5 (s2) ◽  
pp. 1069-1080 ◽  
Author(s):  
Wafaa S. Hassan ◽  
Mervat M. Hosny
Keyword(s):  
Spectrophotometric Method ◽  
Clomiphene Citrate ◽  
Pharmaceutical Preparations ◽  
Conductometric Titration ◽  
Ion Pair ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Colored Complexes ◽  
Standard Deviations

Two accurate, rapid and simple spectrophotometric and conductometric methods were developed for the determination of clomiphene citrate (CMP) and nefazodone HCl (NFZ), the proposed methods depends upon the reaction of ammonium reineckate with the two studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in suitable solvent. The pink colored complexes were determined colorimetrically at 509, 523.6 nm, respectively. Using the conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone in the range 60.02-540.18 and 63.3-443.1 μg mL-1for clomiphene citrate and nefazodone HCl, respectively. While for spectrophotometric method the ranges were 0.2-1.8 and 0.2-1.6 mg mL-1for clomiphene citrate and nefazodone HCl respectively. Various experimental conditions were studied. The results obtained showed good recoveries with relative standard deviations of 0.759 and 0.552%. The proposed procedures were applied successfully to the analysis of these drugs in their pharmaceutical preparations and the results were favourably comparable with the official and reference methods. The molar combining ratio reveal that (1:1) (drug : reagent) ion associates were formed.

scholarly journals Sensitive and Selective Extractive Spectrophotometric Method for the Determination of Hydroxyzine Dihydrochloride in Pharmaceuticals

2019 ◽  
Vol 54 (4) ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiah ◽  
Kanakapura Basavaiah Vinay ◽  
Hosakere Doddarevanna Revanasiddappa
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Ion Pair ◽  
Molar Ratio ◽  
Complexing Agent ◽  
Official Method ◽  
Stoichiometric Ratio ◽  
Experimental Conditions ◽  
Relative Standard

Hydroxyzine dihydrochloride (HDH), a piperazine H1-receptor antagonist and antihistamine, is a rapid acting anxiolytic used principally as an anti-emetic. A sensitive, selective, and precise and accurate spectrophotometric method based on the formation of an ion-pair with orange II (ORG II) as ion-pair complexing agent was developed and validated for the determination of HDH in pharmaceuticals. The chloroform-extractable ion-pair complex exhibited an absorption maximum at 480 nm. Optimization of different experimental conditions is described. Beer’s law is obeyed in the range of 1.5-15 μg mL-1 with an apparent molar absorptivity value of 2.07 x 104 L mol-1 cm-1 and Sandell’s sensitivity value of 0.0216 μg cm-2. The limit of detection (LOD) and limit of quantification (LOQ) are 0.14 and 0.41 μg mL-1, respectively. A Job’s plot of absorbance versus molar ratio of HDH to ORG II indicated (1:2) stoichiometric ratio. Within- and between-day relative standard deviations at three different concentration levels were < 3%. The developed method was successfully applied to commercial tablets. The results obtained were in good agreement with those obtained using the official method. No interference was encountered from co-formulated substances. Recoveries were 96-109 %.

scholarly journals Generic Nonextractive Spectrophotometric Method for Determination of 4-Quino-Naphthollone Antibiotics by Formation of Ion-Pair Complexes with -Naphthol

2006 ◽  
Vol 89 (2) ◽  
pp. 334-340 ◽  
Author(s):  
Ibrahim A Darwish ◽  
Ibrahim H Refaat ◽  
Hassan F Askal ◽  
Mostafa A Marzouq
Keyword(s):  
Spectrophotometric Method ◽  
Dosage Forms ◽  
Ion Pair ◽  
Water Soluble ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Sulfuric Acid Medium ◽  
Quinolone Antibiotics ◽  
Relative Standard

Abstract This paper describes the development of a generic spontaneous nonextractive spectrophotometric method for determination of 13 pharmaceutically important 4-quinolone antibiotics. The method was based on the formation of yellow-colored water-soluble ion-pair complexes between 2% (w/v) -naphthol reagent and each of the studied drugs in sulfuric acid medium at room temperature. The formed ion-pair chromogens have maximum absorption peaks in the range of 365391 nm. The concentrations of the reagents and the experimental conditions affecting the reaction were optimized. Under the optimum conditions, linear relationships with good linear coefficients (0.99870.9995) were found between the absorbance and concentration of the investigated drugs in the range of 10350 g/mL. The assay limits of detection and quantitation were 19.9 and 3.432.9 g/mL, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the analysis of the investigated drugs in pure and pharmaceutical dosage forms with good accuracy and precision; the percentages of label claim ranged from 97.8102.8 0.351.60%. The results obtained by the proposed spectrophotometric method were comparable with those obtained by the official or reported methods. The proposed method is superior to all the previously reported ion-pair formation-based methods in terms of simplicity because it did not involve extraction procedures for the ion-pair complex. Therefore, this method might be recommended for routine use in quality control laboratories for analysis of the investigated 4-quinolone antibiotics in their pure forms, as well as in pharmaceutical dosage forms.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-VISIBLE SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF DULOXETINE

2019 ◽  
pp. 27-31
Author(s):  
LIPSA SAMAL ◽  
AMARESH PRUSTY
Keyword(s):  
Spectrophotometric Method ◽  
Spectroscopic Method ◽  
Solvent System ◽  
Spectrophotometric Analysis ◽  
Thiophene Derivative ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop and validate a simple UV spectroscopic method for the determination of duloxetine, which is a thiophene derivative and a selective neurotransmitter reuptake inhibitor for serotonin, norepinephrine, and to lesser degree dopamine. Methods: The UV Spectrophotometric analysis was performed using Shimadzu UV-1800 and Shimadzu UV-1700 spectrophotometer by using solvent system acetonitrile and water in the ratio of 8:2. Detection was performed at a wavelength of 290 nm. Method validation was carried out according to ICH Q2R1 guidelines by taking the parameters linearity, accuracy, precision, ruggedness, and robustness, LOD and LOQ. Results: The UV Spectrophotometric method was found linear in the range of 10-50 μg/ml. The method was rugged and robust with % relative standard deviation less than 2. The extraction recoveries were found to be higher than 99% in all experimental conditions. Conclusion: Based upon the performance characteristics, the proposed method was found accurate, precise and rapid and suitable for the determination of Duloxetine for routine analysis.

Atomic Absorption Spectrophotometric Method for Determination of Polydimethylsiloxane Residues in Pineapple Juice: Collaborative Study

1990 ◽  
Vol 73 (5) ◽  
pp. 721-723
Author(s):  
Robert D Parker
Keyword(s):  
Nitrous Oxide ◽  
Atomic Absorption ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Atomic Absorption Spectrophotometry ◽  
Pineapple Juice ◽  
Absorption Spectrophotometry ◽  
Relative Standard ◽  
Standard Deviations

Abstract An atomic absorption spectrophotometric method for determination of polydimethylsiloxane (PDMS) residues In pineapple juice was collaboratively studied by 9 laboratories. PDMS residues are extracted from pineapple Juice with 4- methyl-2-pentanone and the extracted silicone Is measured by atomic absorption spectrophotometry using a nitrous oxide/ acetylene flame. Collaborators analyzed 5 samples Including 1 blind duplicate. Reproducibility relative standard deviations (RSDR) were 13.1% at 31 ppm, 6.9% at 18 ppm, 14.8% at 7.9 ppm, and 16.1 % at 4.9 ppm PDMS. The method has been approved Interim official first action by AOAC.

Spectrophotometric Determination of Cyclamate in Soft Drinks and Desserts: Complementary Collaborative Study

1988 ◽  
Vol 71 (6) ◽  
pp. 1212-1214
Author(s):  
Anna-Maija K SJÖBERG
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Soft Drink ◽  
Collaborative Study ◽  
Soft Drinks ◽  
Food Control ◽  
Average Recovery ◽  
Relative Standard ◽  
Standard Deviations

Abstract Fifteen official food control laboratories participated in a collaborative study of a spectrophotometric method to determine cyclamate in a soft drink and a dessert at concentrations of 90-311 mg/L and 202-526 mg/kg, respectively, with blind duplicates and a blank. Average recovery from the soft drink was 97.5%, and from the dessert, 98.6%. Reproducibility relative standard deviations were 4.7-6.5% and 6.9-8.5%, respectively. The outlier percentage was 5.5%. This study complements an earlier work by leading Nordic food laboratories and was designed according to the latest recommendations. The results of this study were compared with those of the earlier collaborative study and with general collaborative results obtained by AOAC.

scholarly journals A New Spectrophotometric Method for Determination of Selenium in Cosmetic and Pharmaceutical Preparations after Preconcentration with Cloud Point Extraction

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Mohammad Hosein Soruraddin ◽  
Rouhollah Heydari ◽  
Morteza Puladvand ◽  
Mir Mehdi Zahedi
Keyword(s):  
Cloud Point ◽  
Spectrophotometric Method ◽  
Cloud Point Extraction ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Samples ◽  
Relative Standard ◽  
Replicate Measurements ◽  
Triton X ◽  
Preconcentration Method

A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL-1; the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL-1of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.

scholarly journals Single-Laboratory Validation of a Method for the Determination of c-Phycocyanin and Allophycocyanin in Spirulina (Arthrospira) Supplements and Raw Materials by Spectrophotometry

2008 ◽  
Vol 91 (3) ◽  
pp. 524-529 ◽  
Author(s):  
Noritaka Yoshikawa ◽  
Amha Belay
Keyword(s):  
Validation Study ◽  
Spectrophotometric Method ◽  
Raw Materials ◽  
Relative Standard ◽  
Standard Deviations ◽  
Test Materials ◽  
Single Laboratory

Abstract A single-laboratory validation study was conducted for a 2-wavelength spectrophotometric method for the determination of c-phycocyanin (cPC) and allophycocyanin (aPC) in Spirulina supplements and raw materials. The absorption maxima of cPC and aPC are at 620 and 650 nm, respectively. The concentrations of the analytes were calculated from measurement of absorbance at 2 wavelengths. This method provided linear responses for cPC and aPC in the range of 25250 g/mL. Duplicate determinations of cPC and aPC in 4 different test materials on 5 different days resulted in relative standard deviations of 0.31.0 and 1.01.5 for cPC and aPC, respectively. Recoveries were 99.2102.4 and 100.0104.0 for cPC and aPC, respectively. The results were satisfactory for the determination of cPC and aPC in Spirulina supplements.

scholarly journals Highly Sensitive Spectrofluorimetric Determination of Ephedrine Hydrochloride in Pharmaceutical Preparations

2006 ◽  
Vol 89 (5) ◽  
pp. 1263-1267 ◽  
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Good Precision ◽  
Experimental Conditions ◽  
Ephedrine Hydrochloride ◽  
Highly Sensitive ◽  
Relative Standard ◽  
Spectrofluorimetric Determination

Abstract A sensitive and specific spectrofluorimetry method was developed and validated for the quantification of ephedrine (EP) in pharmaceutical preparations. The method is based on the fluorescent enhancing reaction of EP with 7-chloro-4-nitrobenzofurazan (NBD-CI; derivatization reagent), in borate buffer of pH 9 to yield a yellow, fluorescent product. Under these experimental conditions, the derivatized product of EP had excitation and emission wavelength maxima at 458 and 516 nm, respectively. The linear range of this method was 202500 ng/mL. The detection limit was 7.3 ng/mL EP. Intra- and interday precisions of the assay at 3 concentrations within this range were 0.0371.77%. The low relative standard deviation values indicate good precision, and high recovery values indicate excellent accuracy of the method. The proposed method was applied to the determination of the examined drugs in pharmaceutical formulations, and the results indicate that the method is equally as accurate, precise, and reproducible as the official method.

scholarly journals Spectrophotometric method for determination of ranitidine hydrochloride in bulk and in pharmaceutical preparation using ninhydrin

2020 ◽  
Vol 11 (4) ◽  
pp. 291-297
Author(s):  
Hutaf Mustafa Baker ◽  
Hussam Ahmad Alsaoud ◽  
Hamzeh Mohamad Abdel-Halim
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Limit Of Quantification ◽  
Ranitidine Hydrochloride ◽  
Relative Standard ◽  
Reproducible Method

A simple, sensitive and reproducible method for the determination of ranitidine hydrochloride in pharmaceutical preparations was investigated. This spectrophotometric method was based on the formation of a deep red color product with ninhydrin in basic media and the absorbance measured at λmax = 480 nm. The reaction occurs at 45 °C with pH = 10 having a contact time of 38 minutes. Under the optimum conditions, Beer’s Law is obeyed in the concentration range of 8.98×103 - 9.90×104 µg/L. The coefficient of correlation was found to be 0.999 for the obtained method with molar absorptivity of 3.05×103 L/mol.cm. The calculated Sandell’s sensitivity is 0.108 μg/cm2. The limit of detection and limit of quantification are 0.0997 and 0.3023 µg/mL, respectively. The low values of the percentage relative standard deviation and percentage relative error indicate the high precision and the good accuracy of the proposed method. The stoichiometry of the reaction is determined and found to be 1:4 (Ranitidine hydrochloride:Ninhydrin). The initial rate method confirmed that this reaction is first order one.

scholarly journals Simultaneous Determination of Codeine and Pyridoxine in Pharmaceutical Preparations by First-Derivative Spectrofluorimetry

2002 ◽  
Vol 85 (4) ◽  
pp. 861-868 ◽  
Author(s):  
Antonio Molina-Díaz ◽  
Natividad Ramos-Martos ◽  
Alberto Navalón ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Ascorbic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Emission Spectra ◽  
Pharmaceutical Formulations ◽  
Native Fluorescence ◽  
First Derivative ◽  
Relative Standard ◽  
Standard Deviations

Abstract A method for the simultaneous determination of codeine and pyridoxine was developed, based on the measurement of their native fluorescence signals, by using first-derivative spectrofluorimetry to resolve the mixture. Codeine was measured at λem = 309 nm, and pyridoxine was measured at λem = 450 nm. Instrumental parameters were optimized, and the emission spectra were recorded between 275 and 475 nm, at λex = 255 nm and excitation and emission slit widths of 2.5 and 10 nm, respectively. Systematic studies on the influence of species usually present along with the analytes (such as caffeine, ascorbic acid, paracetamol, and thiamine) were also performed. The calibration graphs were linear over the ranges of 0.5–7.0 and 0.1–1.0 μg/mL for codeine and pyridoxine, respectively, and the relative standard deviations (n = 10) were about 3%. The method was successfully applied to the determination of codeine and pyridoxine in solutions of synthetic mixtures and in synthetic and semisynthetic pharmaceutical formulations.

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