scholarly journals Rapid and Sensitive Spectrophotometric Method for the Determination of the Trace Amount of Thallium (III) in Water and Urine Samples by New Oxidative Coupling Reaction

2019 ◽  
Vol 53 (4) ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Naef Ghllab Saeed Al-Tayar ◽  
Anantharaman Shivakumar ◽  
Ashwinee Kumar Shresta ◽  
Avinash K. Gowda

A very simple, sensitive and fairly selective direct spectrophotometric method is presented for the rapid determination of thallium(III) at trace level. The method is based on the oxidation of 2-hydrazono-3-methyl-2,3-dihydrobenzo[d]thiazole hydrochloride (MBTH) by thallium(III) in phosphoric acid medium to form a diazoniumcation, which couples immediately with 10,11-dihydro-5Hdibenzo[b,f]azepine (IDB) at room temperature giving a blue colored species having a maximum absorption at 660 nm. The reaction conditions and other important analytical parameters were optimized.The calibration curve was found to be linear over the range of 0.1-4 μg/mL with molar absorptivity of 4.5 × 104 L mol- cm-1 and Sandell’s sensitivity of 0.00454 μg cm-2. The relative standard deviation and limit of detection have been found to be 0.58% and 0.0147 μg/mL respectively. Almost all common anions and cations are found notto interfering in matrix level of the analytical process. The method has been successfully applied for the determination of thallium(III) in synthetic standard mixtures, water and human urine samples. The performance of proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.    

2009 ◽  
Vol 6 (4) ◽  
pp. 1153-1163 ◽  
Author(s):  
P. Nagaraja ◽  
N. Ghllab Saeed Al-Tayar ◽  
A. Shivakumar ◽  
A. K. Shresta ◽  
A. K. Gowda

A novel, simple, rapid, sensitive and selective method has been proposed for the trace determination of thallium by spectrophotometric detection. This method is based on the oxidation of MBTH (3-methyl-2-benzothiazolinone hydrazone hydrochloride) by thallium(III) to form diazonium cation, which couples with IPH (Imipramine hydrochloride) in phosphoric acid medium at room temperature giving a blue colored species having a maximum absorption at 635 nm. The reagents and manifold variables influences on the sensitivity were investigated and the optimum reaction conditions have been established. The calibration curve was found to be linear over the range 0.1-5 μg mL-1with the molar absorptivity and Sandell’s sensitivity of 2.9x104L mol-1cm-1, 0.0071 μg cm-2respectively. The tolerance limit of the method towards various ions usually associated with thallium has been detected. The relative standard deviation for five replicate determination of 2μg mL-1thallium was 0.47%. The method has been successfully applied for the determination of thallium(ІΙΙ) and thallium(I) in synthetic, standard reference materials, water and urine samples with satisfactory results. The performance of the proposed method was evaluated in terms of student’st-test and variance ratioF-test, to find out the significance of proposed method over the reported methods.


2011 ◽  
Vol 8 (4) ◽  
pp. 1528-1535 ◽  
Author(s):  
F. Nekouei ◽  
Sh. Nekouei

A simple, fast, reproducible and sensitive method for the flotation- spectrophotometric determination of Al3+is reported. The apparent molar absorptivity (ε) of the ion associate was determined to be 8.35×104L mol-1cm-1. The calibration curve was linear in the concentration range of 1.0-50 ng mL-1of Al3+with a correlation coefficient of 0.9997. The limit of detection (LOD) was 0.621 ng mL. The relative standard deviation (RSD) at 10 and 30 ng mL-1of aluminium were 1.580 and 2.410% (n=7) respectively. The method was applied for measuring the amount of aluminium in water samples.


2016 ◽  
Vol 11 (2) ◽  
pp. 3540-3551
Author(s):  
Taghreed A. Mohammed ◽  
Mona A. Mohamed

A selective and new spectrophotometric method is described for determination of three antiepileptic drugs; namely lamotrigine (LAM), gabapentin (GAB), and oxcarbazepine (OXC) in drug substances and in drug products using vanillin reagent as the chromogenic agent. The method is based on a coupling reaction between the cited drugs and vanillin reagent in acidic condition. Under optimized conditions, the yellow colored products were measured at 405, 396, and 400 nm respectively. Beer’s law was obeyed at (0.4 – 10), (0.1-10), and (0.5-11) μg/mL, and  the calculated molar absorptivity values are 2.52 x 104, 1.74 x 104, and 2.54 x 104 L/mol/cm for LAM, GAB, and OXC respectively. Sandell sensitivity, the limit of detection (LOD) and limit of quantification (LOQ) were calculated. No interference was observed from common additives found in drug products. The presented method was validated according to ICH guidelines. Statistical comparison of the results was performed using Student's t-test and F-ratio at 95% confidence level, and there was no significant difference between the reference and proposed method with regard to accuracy and precision. The method offers the advantages of rapidity, simplicity and sensitivity and low cost and can be easily applied to resource poor settings without the need for expensive instrumentation and reagents.


2020 ◽  
Vol 11 (4) ◽  
pp. 291-297
Author(s):  
Hutaf Mustafa Baker ◽  
Hussam Ahmad Alsaoud ◽  
Hamzeh Mohamad Abdel-Halim

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.


2009 ◽  
Vol 6 (4) ◽  
pp. 1233-1239 ◽  
Author(s):  
J. Saminathan ◽  
A. S. Sankar ◽  
K. Anandakumar ◽  
T. Vetrichelvan

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%.


2019 ◽  
Vol 10 (2) ◽  
pp. 1420-1423 ◽  
Author(s):  
Amal H. Mhemeed

Easy, the accurate, sensitive spectrophotometric method used to determine Benzocaine in a pure and pharmaceutical preparation. The proposed method depends on using Promethazine hydrochloride as a reagent. Where it depends on oxidative coupling reaction of benzocaine by cerium ammonium sulphate with promethazine hydrochloride in the presence of hydrochloric acid to form green dye product, lmax 615 nm. Beers law is obeyed in the concentration of (5 –300 µg.ml-1). The molar absorptivity is (1.77 * 10 3) L.mol -1.cm-1, a sandal sensitivity of (0.0098) µq.cm-2 and RSD (± 0.56 %). The method gave a successful determination for benzocaine in a pharmaceutical preparation.


2020 ◽  
Vol 17 (3) ◽  
pp. 0780
Author(s):  
Takleef Sallal ◽  
Sumayha Abbas

Rapid, reproducible and accurate method has been developed for the assay for of mebendazol (MBZ) residual assay. The method is based on alkaline hydrolysis of MBZ with sodium hydroxide then oxidation with N-bromosuccinimide (NBS) followed by coupling with 4-Bromoaniline (4-BA) to yield a highly colored product absorbed at maximum 434 nm. Regression analysis of linearity range was found (0.6-2.8) µg.ml-1.  The optimum conditions that affect the oxidation were studied. The developed method was found to be precise with mean value of relative standard deviation (1.153- 1.303) and accurate with relative error (-0.5940-1.7821) .The calculated molar absorptivity and sandal sensitivity values of (29825 L.mol-1.cm-1), 0.0099 µg.cm-2 respectively.  The limit of detection and limit of quantitation were of 0.04696, 0.156548 µg.ml-1 respectively .The suggested method showed good recovery with a mean value of 100.77% for analysis of dosage forms.


2019 ◽  
Vol 24 (4) ◽  
pp. 40
Author(s):  
Aisha A. Abd ◽  
Ali I. Khaleel ◽  
, Faiez M. Hamed

A simple, rapid and sensitive spectrophotometric method for determination of sulphadiazine (SDZ) in aqueous solution is described. The method iis based on the oxidation of SDZ by potasium Periodate, and coupling with ortho-amino phenol to give a violet colour of  maximum absorbaance at 532 nm. Beer's law is obeyed over the concentration range of 5-40 µg /ml of SDZ with a (R2=0.9980) and molar absorptivity 5581.6 L.mol-1.cm-1  and a relative error in the range of - 0.06 - 2.3  % and a relative standard deviation of not more than 0.31 %. The composition of the resulting product is also investigated and it is found to be1:1. The method is successfully applied for the determinatiion of SDZ in pure and pharmaceutical dosage forms, with recovery of noot less than 101.1%.   http://dx.doi.org/10.25130/tjps.24.2019.070


2007 ◽  
Vol 4 (2) ◽  
pp. 173-179 ◽  
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar

A simple spectrophotometric method is proposed for the determination of zidovudine(ZDV) in bulk drug and in pharmaceutical preparations. The method is based on the oxidation of ZDV by a known excess of oxidant N-bromosuccinimide (NBS), in buffer medium of pH 1.5, followed by the estimation of unreacted amount of oxidant with metol and sulphanilic acid. The reacted oxidant corresponds to the amount ZDV. The purple-red reaction product absorbs maximally at 530 nm and Beer’s law is obeyed over a range 5 to 75 μg mL-1. The apparent molar absorptivity is calculated to be 5.1×103L mol-1cm-1, and the corresponding Sandell sensitivity value is 0.052 μg cm-2. The limit of detection and quantification are found to be 0.90 and 2.72, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The method was successfully applied to the assay of ZDV in tablet/capsule preparations and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common tablet/capsule excipients. The accuracy of the method was further ascertained by performing recovery studies via standard-addition method.


2010 ◽  
Vol 7 (4) ◽  
pp. 1612-1620 ◽  
Author(s):  
M. Keyvanfard ◽  
N. Abedi

A new, simple, sensitive and selective kinetic spectrophotometric method was developed for the determination of ultra trace amounts of vanadium(V). The method is based on the catalytic effect of vanadium(V) on the oxidation of malachite green oxalate (MG) by bromate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of malachite green oxalate (MG) at 625 nm with a fixed-time method. The decrease in the absorbance of MG is proportional to the concentration of vanadium(V) in the range of 1-100 ng/mL with a fixed time of 0.5-2 min from the initiation of the reaction. The limit of detection is 0.71 ng/mL of vanadium(V). The relative standard deviation for the determination of 5, 30, 50 ng/mL of vanadium(V) was2.5% 2.6%, 2.4% and respectively. The method was applied to the determination of vanadium(V) in water samples.


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