scholarly journals Spectrophotometric Determination of Bismuth(III) with Arsenazo(III) Reagent in Water samples and Veterinary Preparation

2013 ◽  
Vol 10 (3) ◽  
pp. 986-996
Author(s):  
Baghdad Science Journal
Keyword(s):  
Water Samples ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Water Soluble ◽  
Arsenazo Iii ◽  
Solution Ph ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Composite Mixture

A simple , sensitive and accurate spectrophotometric method for the trace determination of bismuth (III) has been developed .This method is based on the reaction of bismuth (III) with arsenazo(III) in acid solution (pH=1.9) to form a blue water soluble complex which exhibits maximum absorption at 612nm .Beer's law is obeyed over the concentration range of 2-85 ?g bismuth (III) in a final volume of 20 mL( i.e. 0.1 – 4.25?g.mL-1) with a correlation coefficient of (0.9981) and molar absorptivity 1.9×104 L.mol-1.cm-1 . The limit of detection (LOD) and the limit of quantification (LOQ) are 0.0633 and 0.0847 ?g.mL-1 , respectively . Under optimum conditions,the stoichiometry of the reaction between bismuth (III) and arsenazo(III) reagent was found to be 1:2. The recoveries were obtained in the range of 98.9 - 100.0% and a relative standard deviation of ±0.59 to ±2.73% depending on the concentration level of bismuth. The effect of interferences by a number of common cations and anions in the presence of composite mixture has been studied .The proposed method has been applied successfully for determination of bismuth in water samples and veterinary preparation .

scholarly journals Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

scholarly journals POSSIBILITY OF THE SPECTROPHOTOMETRIC DETERMINATION OF EUROPIUM BY MEANS OF ARSENAZO III

2013 ◽  
Vol 12 (2) ◽  
pp. 93-99 ◽  
Author(s):  
Jozef Uhrovčík ◽  
Monika Gyeváthová ◽  
Juraj Lesný
Keyword(s):  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Model Solution ◽  
Arsenazo Iii ◽  
Complexing Agent ◽  
Acceptable Range ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Interfering Ions

Abstract The concentration of Eu(III) cations in model aqueous solutions can be quantified by means of Arsenazo III reagent. Absorbance of the solution was measured at the wavelength λmax = 655 nm. Molar absorptivity reached the value ε655 = 5.5±0.2 · 104 cm-1 mol-1 · dm3. Beer's law was obeyed in the range from 0 to 2 mg · dm-3 Eu(III). The value of limit of detection was established by application of 3σ approach and reached the value of 20.9 μg · dm-3. Repeatability of analysis expressed by relative standard deviation does not exceed the value of ± 8% and apparent recovery lay in acceptable range from 91 to 106 %. Stoichiometry between Eu(III) and Arsenazo III in media of relevant solution was 1:1. The absorbance of the solutions within the linear range of the proposed method maintained a constant value for 60 minutes. Described procedure can be utilized to determination of Eu(III) concentration in real samples, but it is necessary eliminate interfering ions. Cations like La(III), Sm(III), Th(IV), U(VI) and complexing agent EDTA cause significant error at the determination of Eu(III) in model solution. Presented spectrophotometric method could be applied for the determination of europium in the minerals and water samples, however after a suitable separation and preconcentration of target analyte.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

scholarly journals EXTRACTION AND DETERMINATION OF TEBUCONAZOLE IN ENVIRONMENTAL SAMPLES FROM THE CITY OF KERBALA, IRAQ AND IN ITS FORMULATION USING HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Percentage Recovery ◽  
Relative Standard

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.

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 Direct Spectrophotometric Determination of Glimepiride in Pure Form And Pharmaceutical Formulations Using Bromocresol Purple

2018 ◽  
Vol 15 (2) ◽  
pp. 6186-6198
Author(s):  
Abdul Aziz Ramadan ◽  
Souad Zeino
Keyword(s):  
Limit Of Detection ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Bromocresol Purple ◽  
Reaction Conditions ◽  
Reagent Blank ◽  
Limit Of Quantification ◽  
Relative Standard

A simple, direct and accurate spectrophotometric method has been developed for the determination of Glimepiride (GLM) in pure and pharmaceutical formulations by complex formation with bromocresol purple (BCP). The method involves the formation of a yellow ion-pair complex between BCP with glimepiride at pH<3,8; after reacting GLM with Na2CO3 to give C24H33N4H+O5NaS which is extracted by chloroform. The formed complex [GLM]:[ BCP] was measured at lmax 418 nm against the reagent blank prepared in the same manner. Variables were studied in order to optimize the reaction conditions. Molar absorptivity (e) for complex was  20600  L.mol-1.cm-1. Beer’s law was obeyed in the concentration range of  1.226 – 46.608   mg.mL-1 in present of 5.0x10-4 mol/l of BCP with good correlation coefficient (R2= 0.9997). The relative standard deviation did not exceed 3.6%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.15 and 0.46 mg.mL-1, respectively. The proposed method was validated for specificity, linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ)  and robustness. The developed method is applicable for the determination of GLM in  pure and different dosage forms with average assay of 98.8 to 102.0% and the results are in good agreement with those obtained by the  RP-HPLC reference method.  

Utility of π-acceptor reagents for spectrophotometric determination of sulphonamide drugs via charge-transfer complex formation

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Faten Nour El-Dien ◽  
Gehad Mohamed ◽  
Eman Frag
Keyword(s):  
Charge Transfer ◽  
Standard Deviation ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Official Method ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Chloranilic Acid ◽  
Relative Standard

AbstractA simple, sensitive and accurate spectrophotometric method for the determination of sulphonamides (sulphamethoxazole (SMZ), sulphaguanidine (SGD), sulphaquinoxaline sodium (SQX), sulphametrole (SMR), and sulphadimidine sodium (SDD)) has been developed. The charge-transfer reactions between sulphonamides as n-electron donors and 7,7,8,8-tetracyanoquinodimethane (TCNQ), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), and 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone (chloranilic acid, p-CLA) as π-acceptors resulting in highly coloured complexes were studied. Experimental conditions for these CT reactions were carefully optimised. Beer’s law is valid over the concentration ranges from 4–280 µg mL−1, 4–260 µg mL−1, 4–200 µg mL−1, and 4–200 µg mL−1 of SMZ, SGD, SQX, and SDD using DDQ reagent, respectively. While the calibration curves are linear in the concentration ranges from 4–180 µg mL−1, 4–80 µg mL−1, 4–60 µg mL−1, 4–180 µg mL−1, and 4–60 µg mL−1 of SMZ, SGD, SQX, SMR, and SDD, respectively, using TCNQ reagent and from 4–380 µg mL−1 and 4–300 µg mL−1 of SQX and SDD, respectively, using p-CLA reagent, respectively. Different analytical parameters, namely molar absorptivity (ε), standard deviation, relative standard deviation, correlation coefficient, limit of detection, and limit of quantification, were calculated. The results obtained by the proposed methods are in good agreement with those obtained by the official method as indicated by the percent recovery values.

scholarly journals Simple UV Spectrophotometric Method for the Determination of Fluvastatin Sodium in Bulk and Pharmaceutical Formulations

2009 ◽  
Vol 6 (4) ◽  
pp. 1233-1239 ◽  
Author(s):  
J. Saminathan ◽  
A. S. Sankar ◽  
K. Anandakumar ◽  
T. Vetrichelvan
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Regression Line ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Good Precision ◽  
Limit Of Quantification ◽  
Relative Standard

A simple and cost effective spectrophotometric method is described for the determination of fluvastatin sodium in pure form and in pharmaceutical formulations. When the drug reacts with sodium hydroxide shows absorption maximum at 304 nm and obeys beer's law in the concentration range 5-25 µg mL-1. The absorbance was found to increase linearly with increasing concentration of FVS, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=5). The apparent molar absorptivity and sandell sensitivity were 1.1905×104and 0.0368844 µg cm-2cm respectively. The slope and intercept of the equation of the regression line are 0.027112 and 0.003539 respectively. The limit of detection and limit of quantification was found to be 0.0811 µg mL-1& 0.2460 µg mL-1. The validity of the described procedure was assessed. Statistical analysis of the result has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of FVS in pharmaceutical formulations without any interference from common excipients. The relative standard deviations were ≤ 0.937%, with recoveries of 98.60% -101.70%.

scholarly journals Vortex Assisted Liquid-Liquid Microextraction with Back Extraction of Repaglinide, Glibenclamide and Glimepiride in Water Samples

2021 ◽  
Vol 50 (5) ◽  
pp. 1297-1307
Author(s):  
Sohaib Jumaah Owaid Luhaib ◽  
Noorfatimah Yahaya ◽  
Anas Alshishani ◽  
Maizatul Najwa Jajuli ◽  
Mazidatulakmam Miskam
Keyword(s):  
Water Samples ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Aqueous Sample ◽  
Back Extraction ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Liquid Microextraction

A new analytical method based on vortex-assisted liquid-liquid microextraction with back extraction (VALLME-BE) coupled with high performance liquid chromatography was developed for the simultaneous determination of antidiabetic drugs; repaglinide, glibenclamide, and glimepiride in water samples. Chromatographic separation was achieved using C18 column (250 × 4.6 mm × 5 µm) and methanol-phosphate buffer (pH3.7) in the ratio of 70:30 v/v as a mobile phase at a flow rate of 1 mLmin-1. VALLME-BE was performed using 200 μL of n-octane dispersed into the aqueous sample (10 mL) with the aid of vortexing agitation. Then, the analytes were back-extracted from the organic solvent to 0.05 M NaOH (40 µL). Under these conditions, enrichment factor of 155-fold was achieved. The developed VALLME-BE method showed excellent linearity in the range of 30 to 1000 µgL-1 with limit of detection (LOD) of 0.41-1.66 µgL-1 and limit of quantification (LOQ) of 1.38-5.54. 41-1.66 µgL-1. VALLME-BE was applied for the determination of repaglinide, glibenclamide and glimepiride in water samples with the recoveries ranged from 83-109%. The relative standard deviation for inter-day and intra-day precision was less than 9.9%.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

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