scholarly journals An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

2008 ◽  
Vol 73 (5) ◽  
pp. 569-576 ◽  
Author(s):  
Mohamed Issa ◽  
Mahmoud Nejem ◽  
Monzer Al-Kholy ◽  
Said El-Abadla ◽  
Sobhi Helles ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Diclofenac Sodium ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Drug Substances ◽  
Low Concentrations ◽  
Coefficients Of Variation ◽  
Highly Sensitive ◽  
Aqueous Layer

A highly sensitive indirect atomic absorption spectrophotometric (AAS) method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III). The excess of iron(III) was extracted into diethyl ether and then the iron(II) in the aqueous layer was aspirated into an air-acetylene flame and determined by AAS. The linear concentration ranges were 25-400, 50-500 and 60-600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

scholarly journals Stability-Indicating Micelle-Enhanced Spectrofluorimetric Method For Determination of Tamsulosin Hydrochloride In Dosage Forms.

2015 ◽  
Vol 11 (2) ◽  
pp. 3513-3531 ◽  
Author(s):  
Mona Elsayed Elshahed ◽  
Ibrahim Habib
Keyword(s):  
Fluorescence Intensity ◽  
Sodium Dodecyl ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Forced Degradation ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Highly Sensitive ◽  
Good Agreement

A rapid, simple and highly sensitive spectrofluorimetric method is developed for the determination of Tamsulosin hydrochloride (Tams.HCl) in pharmaceutical formulations. The proposed method is based on investigation of the fluorescence spectral behavior of Tams.HCl in a sodium dodecyl sulphate (SDS) micellar system. In aqueous solution of Tris buffer of pH 7±0.2, SDS causes marked enhancement in the fluorescence intensity of Tams.HCl (about +110%). The fluorescence intensity is measured at 328 nm after excitation at 280 nm and the fluorescence-concentration plots are rectilinear over the range 0.1-1.2 µg ml-1, with lower detection limit of 0.027 µg ml-1 and quantification limit of 0.09 µg ml-1. The method is successfully applied to the analysis of the studied drug in its commercial capsules, and the results are in good agreement with those obtained with the official method. The application of the proposed method is extended to stability studies of Tamsulosin hydrochloride after exposure to different forced degradation conditions, such as acidic, alkaline and oxidative conditions, according to ICH guidelines.

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.

Determination of Cadmium, Copper, and Lead in Sodium Chloride Food Salts by Flame Atomic Absorption Spectroscopy

1986 ◽  
Vol 69 (5) ◽  
pp. 871-873
Author(s):  
M Jesus Alvarez de Eulate ◽  
Rosa Montoro ◽  
Nieves Ybañez ◽  
Miguel De La Guardia
Keyword(s):  
Sodium Chloride ◽  
Atomic Absorption ◽  
Absorption Spectroscopy ◽  
Atomic Absorption Spectroscopy ◽  
Pyrrolidine Dithiocarbamate ◽  
Flame Atomic Absorption Spectroscopy ◽  
Flame Atomic Absorption ◽  
Coefficients Of Variation ◽  
Ammonium Pyrrolidine Dithiocarbamate

Abstract A method for determination of Cd, Cu, and Pb in sodium chloride food salt samples has been developed. It consists of extraction in 4- methj 1-2-pentanonc of the complexes formed with ammonium pyrrolidine dithiocarbamate and further analysis of the extracts by flame atomic absorption spectroscopy. Detection limits in ng/g salt were 0.2 for Cd, 0.7 for Cu, and 10.0 for Pb. The coefficients of variation of 12 independent analyses were 13% for Cd (at a level of 0.4 ppb), 18% for Cu (1.6 ppb), and 5% for Pb (40 ppb). The recoveries were 100 ± 0% for Cd, 115 ± 14% for Cu, and 100 ± 13% for Pb.

scholarly journals Polymeric Matrix Membrane Sensors for Stability-Indicating Potentiometric Determination of Oxybutynin Hydrochloride and Flavoxate Hydrochloride Urogenital System Drugs

2008 ◽  
Vol 91 (6) ◽  
pp. 1318-1330 ◽  
Author(s):  
Mohamed Heba ◽  
Nesrin Ramadan ◽  
Moustafa El-Laithy
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Urogenital System ◽  
Electroactive Materials ◽  
Significant Difference ◽  
Ph Range ◽  
Oxybutynin Hydrochloride ◽  
Flavoxate Hydrochloride

Abstract Four polyvinyl chloride (PVC) matrix membrane electrodes responsive to 2 drugs affecting the urogenital systemoxybutynin hydrochloride (OX) and flavoxate hydrochloride (FX)were developed, described, and characterized. A precipitation-based technique with tungstophosphate (TP) and ammonium reineckate (R) anions as electroactive materials in a PVC matrix with an OX cation was used for electrode 1 and 2 fabrication, respectively. Electrode 3 and 4 fabrication was based on use of the precipitation technique of FX cation with tetrakis (4-chlorophenyl) borate and R anions as electroactive materials. Fast and stable Nernstian responses in the range 1 1021 106 M for the 2 drugs over the pH range 58 revealed the performance characteristics of these electrodes, which were evaluated according to International Union of Pure and Applied Chemistry recommendations. The method was applied to FX and OX in their pharmaceutical formulations and in human plasma samples. The 4 proposed sensors were found to be specific for the drugs in the presence of up to 60 of their degradation products. Validation of the method according to the quality assurance standards showed suitability of the proposed electrodes for use in the quality control assessment of these drugs. The recoveries for determination of the drugs by the 4 proposed selective electrodes were 99.5 0.5, 100.0 0.4, 99.9 0.4, and 100.1 0.4 for sensors 14, respectively. Statistical comparison between the results obtained by this method and the official method of the drugs was done, and no significant difference found.

scholarly journals Spectrofluorometric Determination of Verapamil Hydrochloride in Pharmaceutical Preparations and Human Plasma Using Organized Media: Application to Stability Studies

2006 ◽  
Vol 89 (6) ◽  
pp. 1565-1572 ◽  
Author(s):  
Mohamed Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelsalam
Keyword(s):  
Human Plasma ◽  
Biological Fluids ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Official Method ◽  
Stability Studies ◽  
Verapamil Hydrochloride ◽  
Spiked Human Plasma

Abstract A highly sensitive spectrofluorometric method was developed for the determination of verapamil hydrochloride (VP HCl) in pharmaceutical formulations and biological fluids. The proposed method is based on investigation of the fluorescence spectral behavior of VP HCl in micellar systems, such as sodium dodecyl sulfate (SDS) and β-cyclodextrin (β-CD). In aqueous solutions of borate buffer of pH 9 and 8.5, VP HCl was well incorporated into SDS and β-CD, respectively, with enhancement of its native fluorescence. The fluorescence was measured at 318 nm after excitation at 231 nm. The fluorescence intensity enhancements were 183 and 107% in SDS and in β-CD, respectively. The fluorescence-concentration plots were rectilinear over the range of 0.020.2 and 0.020.25 μg/mL, with lower detection limits of 5.58 × 103 and 3.62 × 103 μg/mL in SDS and β-CD, respectively. The method was successfully applied to the analysis of commercial tablets and the results were in good agreement with those obtained with the official method. The method was further applied to the determination of VP HCl in real and spiked human plasma. The mean % recoveries in the case of spiked human plasma (n 4) was 92.59 3.11 and 88.35 2.55 using SDS and β-CD, respectively, while that in real human plasma (n 3) was 90.17 6.93 and 89.17 6.50 using SDS and β-CD, respectively. The application of the method was extended to the stability studies of VP HCl after exposureto ultraviolet radiation and upon oxidation with hydrogen peroxide.

scholarly journals A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

2008 ◽  
Vol 33 (3) ◽  
pp. 7-12 ◽  
Author(s):  
M. A. Gotardo ◽  
L. S. Lima ◽  
R. Sequinel ◽  
J. L. Rufino ◽  
L. Pezza ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Coefficients Of Variation ◽  
The Common ◽  
Interday Precision ◽  
Sensitive Spectrophotometric Method

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

scholarly journals VISIBLE SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION OF IMATINIB IN BULK AND FORMULATION

2020 ◽  
pp. 63-67
Author(s):  
SMITA KUMBHAR ◽  
VINOD MATOLE ◽  
YOGESH THORAT ◽  
ANITA SHEGAONKAR ◽  
AVINASH HOSMANI
Keyword(s):  
Spectrophotometric Method ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Uv Spectrum ◽  
Colored Complex ◽  
Pharmaceutical Dosage Forms ◽  
Highly Sensitive ◽  
Method Development And Validation ◽  
Development And Validation

Objective: A new, simple, sensitive, precise and reproducible UV visible spectrophotometric method was developed for the determination of Imatinib in pharmaceutical formulations with alizarin. Methods: The method is based on formation of yellow-colored complex. The UV spectrum of Imatinib in methanol showed λ max at 431 nm. Beer’s law is valid in the concentration range of 10-70 μg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness. Results: The method has demonstrated excellent linearity over the range of 10-70 μg/ml with regression equation y =0.013x-0.017 and regression correlation coefficient r2= 0.997. Moreover, the method was found to be highly sensitive with LOD (4.3μg/ml) and LOQ (13.07μg/ml). Conclusion: Based on results the proposed method can be successfully applied for the assay of Imatinib in various pharmaceutical dosage forms.

Atomic Absorption Spectrophotometric Determination of 4-Hydroxy-3-Nitrobenzenearsonic Acid (Roxarsone) in Premixes

1975 ◽  
Vol 58 (5) ◽  
pp. 945-948 ◽  
Author(s):  
Larry J Frahm ◽  
Marven E Albrecht ◽  
J Patrick Mcdonnell
Keyword(s):  
Atomic Absorption ◽  
Ammonium Carbonate ◽  
Atomic Absorption Spectrophotometry ◽  
Electrodeless Discharge ◽  
Absorption Spectrophotometry ◽  
Coefficients Of Variation ◽  
Instrument Response ◽  
Variation Range ◽  
Standard Solution

Abstract Roxarsone (4-hydroxy-3-nitrobenzenearsonic acid) is extracted from the premix with aqueous 1% ammonium carbonate. The extract is filtered, diluted, and analyzed by atomic absorption spectrophotometry, using an air-acetylene flame and an arsenic electrodeless discharge lamp. The instrument response of the sample is compared to that of a standard solution of arsenic trioxide. Recoveries range from 99.7 to 100.4% and coefficients of variation range from 0.35 to 0.63%.

Radioimmunoassay for pregnancy-associated plasma protein A.

1982 ◽  
Vol 28 (1) ◽  
pp. 50-53 ◽  
Author(s):  
M J Sinosich ◽  
B Teisner ◽  
J Folkersen ◽  
D M Saunders ◽  
J G Grudzinskas
Keyword(s):  
Detection Limit ◽  
Amniotic Fluid ◽  
Plasma Protein ◽  
Early Pregnancy ◽  
Twin Pregnancy ◽  
Protein A ◽  
Trophoblastic Disease ◽  
Coefficients Of Variation ◽  
Highly Sensitive

Abstract A specific and highly sensitive radioimmunoassay for determination of pregnancy-associated plasma protein A in human serum is described. The minimum detection limit for this protein was 2.9 micrograms/L. The within- and between-assay coefficients of variation were 4.0 and 4.5%, respectively. The circulating protein was detected within 32 days of conception in eight normal pregnancies and within 21 days in a twin pregnancy. Circulating concentrations in the mother at term were consistently higher (10-fold) than in matched amniotic fluid; none was detected in the umbilical circulation. This protein was also detected in the circulation of patients with hydatiform mole. This assay will permit investigations into the clinical evaluation of measurements of the protein during early pregnancy and trophoblastic disease.

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