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

2006 ◽  
Vol 89 (5) ◽  
pp. 1263-1267 ◽  
Author(s):  
Sevgi Tatar Ulu

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.

2005 ◽  
Vol 2005 (1) ◽  
pp. 1-9 ◽  
Author(s):  
F. A. Nour El-Dien ◽  
M. A. Zayed ◽  
Gehad. G. Mohamed ◽  
Reham G. El-Nahas

Two simple, rapid, and sensitive spectrophotometric methods are proposed for the determination of levodopa (LD). The first method is based on coupling of 4-aminoantipyrine (4-AAP) with one of the dopamine derivatives (LD, CD) to give a new ligand that reacts with copper tetramine complex to give intensely colored chelates. The colored products are quantified spectrophotometrically at 525 and 520 nm for LD and CD, respectively. The optimization of the experimental conditions is described. The method has been used for the determination of19.7–69.0and18.1–54.3μg mL−1of LD and CD, respectively. The accuracy of the method is achieved by the values of recovery (100±0.2%) and the precision is supported by the low standard deviation (SD=0.17–0.59) and relative standard deviation (CV=0.4%–1.54%) values. The second method is based on the formation of ion-pair iodinated inner sphere or outer sphere colored complexes between the LD and triiodide ions at pH 5 and room temperature (23±3°C). This method has been used for the determination of LD within the concentration range39.44–78.88μg mL−1with SD=0.22–0.24and recovery percent=100±0.3%. The sensitivity of the two methods is indicated by Sandell's sensitivity of0.014–0.019g cm−2. The results of the two methods are compared with those of the official method. The interference of common drug additives, degradation products, and excipients was also studied. The proposed methods were applied successfully to the determination of the LD-CD synthetic mixture and Levocare drug. The determination of LD in urine of some schizophrenic patients was applied with good precision and accuracy. The reliability of the methods was established by parallel determinations against the official British pharmacopoeia method.


2020 ◽  
Vol 16 ◽  
Author(s):  
Sheng-Yun Li ◽  
Fang Tian

: A spectrophotometry was investigated for the determination of epsilon aminocaproic acid (EACA) with p-nitrophenol (PNP). The method was based on a charge transfer (CT) complexation of this drug as n-electron donor with π-acceptor PNP. Experiment indicated that the CT complexation was carried out at room temperature for 10 minutes in dimethyl sulfoxide solvent. The spectrum obtained for EACA/PNP system showed the maximum absorption band at wavelength of 425 nm. The stoichiometry of the CT complex was found to be 1:1 ratio by Job’s method between the donor and the acceptor. Different variables affecting the complexation were carefully studied and optimized. At the optimum reaction conditions, Beer’s law was obeyed in a concentration limit of 1~6 µg mL-1. The relative standard deviation was less than 2.9%. The apparent molar absoptivity was determined to be 1.86×104 L mol-1cm-1 at 425 nm. The CT complexation was also confirmed by both FTIR and 1H NMR measurements. The thermodynamic properties and reaction mechanism of the CT complexation have been discussed. The developed method could be applied successfully for the determination of the studied compound in its pharmaceutical dosage forms with a good precision and accuracy compared to official method as revealed by t- and F-tests.


2013 ◽  
Vol 10 (3) ◽  
pp. 1005-1013 ◽  
Author(s):  
Baghdad Science Journal

A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations (tablets) and industrial wastewater samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of tadalafil in true samples.


2006 ◽  
Vol 89 (6) ◽  
pp. 1565-1572 ◽  
Author(s):  
Mohamed Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelsalam

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.


2008 ◽  
Vol 5 (s2) ◽  
pp. 1069-1080 ◽  
Author(s):  
Wafaa S. Hassan ◽  
Mervat M. Hosny

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.


2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mohsen Zeeb ◽  
Mahdi Sadeghi

An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future.


2020 ◽  
Vol 15 (1) ◽  
pp. 21-26
Author(s):  
M.Ye. Blazheyevskiy ◽  
Yu.V. Scrypynets ◽  
A.V. Yegorova ◽  
V.P. Antonovich

The oxidative derivatization method for the indirect spectrofluorimetric determination of Periciazine has been presented. Potassium hydrogenperoxymonosulfate (Oxone ®) is proposed as a derivatizing agent for Periciazine, yielding the strongly fluorescent Periciazine sulfoxide. A highly sensitive, simple and rapid method for determination of the Periciazine by fluorescence of its oxidation product with Oxone ® solution in 0.02 M hydrochloric acid solution (λex = 364 nm; λem = 444 nm) has been developed. The calibration plot is linear in concentration range of 0.05 – 4.00 µg mL -1 . LOQ (10S) is 0.05 µg mL -1 . The possibility of quantitative determination of Periciazine in pharmaceutical preparations (Neuleptil ®, 10 mg capsules and Neuleptil ®, a 30 mL 4 % oral (solution) drops) has been shown RSD < 2.2 % (δ < RSD).


2001 ◽  
Vol 69 (2) ◽  
pp. 151-160
Author(s):  
A. Amin ◽  
H. Saleh

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceutical formulations based on the formation of ion-pair complexes with sudun II (SII), sudan (IV) (SIV) and sudan black B (SBB). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.


2007 ◽  
Vol 90 (4) ◽  
pp. 941-947 ◽  
Author(s):  
Manal Eid ◽  
Amina El-Brashy ◽  
Fatma Aly ◽  
Wael Talaat

Abstract A simple and sensitive fluorometric method for determination of ketorolac tromethamine was studied. The method depends on oxidation of the drug with cerium(IV) and subsequent monitoring of the fluorescence of the induced cerium(III) at em 365 nm after excitation at 255 nm. Different variables affecting the reaction conditions, such as the concentrations of cerium(IV), sulfuric acid concentration, reaction time, and temperature, were carefully studied and optimized. Under the optimum conditions, a linear relationship was found between the relative fluorescence intensity and the concentration of the investigated drug in the range of 0.10.8 g/mL. No interferences could be observed from the excipients commonly present in dosage forms. The proposed method was successfully applied to the analysis of the investigated drug in its pure form, pharmaceutical preparations, and biological fluids with good accuracy and precision. The recoveries for pharmaceutical formulations ranged from 99.8101.0 0.6% for tablets, 98.5101.0 1.0% for ampoules, and 99.0100.5 0.7% for eye drops. The results obtained by the proposed method were satisfactory compared with those obtained by the official method. The recoveries for biological fluids were 99.1100.4 0.7 and 99.0100.0 0.5% for plasma and urine, respectively.


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