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

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.

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.


Author(s):  
DAVID ALEXANDER ◽  
Abdul Rohman

Objective: The aim of this research was to validate inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for quantitative analysis of cadmium (Cd), chromium (Cr), cuprum (Cu), mangan (Mn) and nickel (Ni) in milk products. Methods: The heavy metals in milk were determined using ICP-AES at optimized wavelength. The method was validated by assessing several validation parameters which included linearity and range, accuracy, precision and sensitivity expressed by the limit of detection and limit of quantification. The validated method was then used for the analysis of milks commercially available. Results: ICP-AES for determination of Cd, Cr, Cu, Mn, and Ni was linear over a certain concentration range with a coefficient correlation value of>0.997. The limit of quantification values of Cd, Cr, Cu, Mn, and Ni were 0.0047; 0.0050; 0.0066; 0.0061; and 0.0169 µg/ml, respectively. The precision of analytical method exhibited relative standard deviation (RSD) values of 3.18%; 4.17%; 3.05%; 2.93%; and 4.47% during repeatability test and 5.28%; 5.06%; 3.67%; 3.67%; and 11.17% during intermediate precision of Cd, Cr, Cu, Mn, and Ni respectively. The recoveries of these metals assessed using standard addition method were 92.25; 90.88; 102.87; 94.50; and 86.85%, respectively. Conclusion: ICP-AES offered a reliable and fast method for the determination of heavy metals in milk products. The developed method could be proposed as an official method for determination of heavy metals in milk products.


2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe

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.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.


2010 ◽  
Vol 7 (2) ◽  
pp. 395-402
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Kumar Shrestha

A spectrophotometric method has been proposed for the determination of four phenolic drugs; salbutamol, ritodrine, amoxicillin and isoxsuprine. The method is based on the oxidation of 2, 4- dinitrophenyl-hydrazine and coupling of the oxidized product with drugs to give intensely colored chromogen. Under the proposed optimum condition, beer’s law was obeyed in the concentration range of 2.5-17, 2-29, 4-33 and 5-30 μg/mL for salbutamol, ritodrine, amoxicillin and isoxsuprine respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 0.2, 0.83, 0.09, 0.84 μg/mL and 0.66, 2.79, 0.3 and 2.81 μg/mL in the same order. No interference was observed from common pharmaceutical adjuvants. The ringbom plots and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical dosage forms, which was compared statistically with reference methods by means oft- test andF- test and were found not to differ significantly at 95% confidence level. The procedure is characterized by its simplicity with accuracy and precision.


2011 ◽  
Vol 17 (3) ◽  
pp. 259-267 ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiahf ◽  
Basavaiah Vinay

Quetiapine fumarate (QTF) is an antipsychotic drug belonging to the benzisoxazole derivatives indicated for the treatment of schizophrenia. A sensitive and selective method based on dichloromethane-extractable ion-pair of QTF with calmagite (CGT), which exhibited an absorption maximum at 490 nm, is described. At this wavelength, Beer?s law is obeyed over the concentration range of 3.0 - 30.0 ?g ml-1. The apparent molar absorptivity, limit of detection (LOD) and quantitation (LOQ) values are 1.32 ? 104 l mol-1 cm-1, 0.27 and 0.81 ?g ml-1 respectively. The reaction is extremely rapid at room temperature and the absorbance values remain unchanged upto 19 h. The precision results, expressed as intra-day and inter-day relative standard deviation values, are satisfactory (RSD ? 2.2%). The accuracy is satisfactory as well (RE ? 2.44%). The method was successfully applied to the determination of QTF in pharmaceuticals and spiked human urine with satisfactory results. No interference was observed from common pharmaceutical adjuvants in tablets. Statistical comparison of the results with official method showed an excellent agreement and indicated no significant difference in precision.


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.


Author(s):  
Muchlisyam Muchlisyam ◽  
Sudarmi Sudarmi ◽  
Cindy Caroline

 Objective: Mean centering of ratio spectra method (MCR method) is one of the simplest methods for the determination of drug mixtures. The purpose of this research is to determine the content of theophylline (THEO) and ephedrine HCl (EPH) in tablets by MCR spectra method.Methods: This research was conducted with the MCR method. It was measured at 271 nm for THEO and 257 nm for EPH using 0.1 N HCL as a solution. The calculation was conducted with Matlab application. The analytical characteristics of the method are detection limit, accuracy, precision, and selectivity. Standard addition method was used to increase the concentration of EPH in the sample until it reached the range of calibration concentration.Result: The research has showed that validations for THEO were 100.57% for accuracy, 0.68% for relative standard deviation (RSD), 0.46 μg/mL for limit of detection (LOD), and 1.52 μg/mL for limit of quantification (LOQ). Meanwhile, the validations for EPH are 100.02% for accuracy, 0.07% for RSD, 43.12 μg/mL for LOD, and 143.72 μg/mL for LOQ. The level of THEO is 97.43 ± 0.17% and the level of EPH is 101.36 ± 0.25% for brand one’s tablet. Meanwhile, brand two’s tablet contains 98.72 ± 0.14% of THEO and 103.62 ± 0.23% of EPH.Conclusion: MCR ultraviolet spectrophotometric method can be used to determine the content of THEO and EPH in tablets and meets the detection limit, accuracy, precision, and selectivity.


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.


2019 ◽  
Vol 54 (4) ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiah ◽  
Kanakapura Basavaiah Vinay ◽  
Hosakere Doddarevanna Revanasiddappa

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 %.


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