Electrochemical behavior of disopyramide and its adsorptive stripping determination in pharmaceutical dosage forms and biological fluids

2010 ◽  
Vol 75 (6) ◽  
pp. 685-702 ◽  
Author(s):  
Funda Öztürk ◽  
Ibrahim Hüdai Taşdemir ◽  
Zehra Durmuş ◽  
Esma Kiliç
Keyword(s):  
Electrochemical Reduction ◽  
Electrochemical Behavior ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Direct Determination ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Square Wave ◽  
Standard Rate

Electrochemical behavior of disopyramide (DPA) and optimum conditions to its quantitative determination were investigated using voltammetric methods. Some electrochemical parameters such as diffusion coefficient, surface coverage of adsorbed molecules, electron transfer coefficient, standard rate constant and number of electrons were calculated using the results of cyclic and square-wave voltammetry. All studies were based on the quasi-reversible and adsorption-controlled electrochemical reduction signal of DPA at about –1.60 V vs Ag|AgCl at pH 10.0 in Britton–Robinson buffer. This adsorptive character of molecule was used to develop fully validated, new, rapid, selective and simple square-wave cathodic adsorptive stripping voltammetric (SWCAdSV) method to the direct determination of DPA in pharmaceutical dosage forms and biological samples without time-consuming steps prior to drug assay. Peak current of electrochemical reduction of DPA was found to change linearly with the concentration in the range from 7.15 × 10–8 mol l–1 (0.024 mg l–1) to 1.43 × 10–6 mol l–1 (0.49 mg l–1). Limit of detection (LOD) and limit of quantification (LOQ) were found to be 5.65 × 10–8 mol l–1 (0.019 mg l–1) and 1.88 × 10–7 mol l–1 (0.064 mg l–1), respectively. The method was successfully applied to assay the drug in tablets, human serum and human urine with good recoveries at about 100%.

Lacidipine: review of analytical methods developed for pharmaceutical dosage forms and biological fluids

Bioanalysis ◽  
2021 ◽  
Author(s):  
Sai Tejasvini Chebrolu ◽  
Lalit Kumar ◽  
Ruchi Verma
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Ultra Violet ◽  
Analytical Techniques ◽  
Dosage Forms ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms

Lacidipine (LAC) is a calcium antagonist used in the treatment of hypertension. It is a lipophilic drug containing dihydropyridine ring that is responsible for the activity. This review article gives an overview of various analytical techniques proposed for the determination of LAC in pharmaceutical dosage forms, in pure form, in biological fluids and to determine characteristics of LAC in modified release dosage forms. Ultra violet/visible spectrophotometric, spectroflourimetric, high performance liquid chromatography, high performance thin layer chromatography, electro-analytical, bioanalytical and miscellaneous methods such as microbiological assay, X-ray diffraction, differential scanning calorimetry, were discussed. Various parameters such as system suitability, selectivity, linearity, precision, accuracy, limit of detection, limit of quantification and robustness have been discussed for the employed methods.

Electrochemical oxidation of atorvastatin and its adsorptive stripping determination in pharmaceutical dosage forms and biological fluids

2011 ◽  
Vol 76 (12) ◽  
pp. 1633-1649 ◽  
Author(s):  
Dilek Eskiköy ◽  
Zehra Durmuş ◽  
Esma Kiliç
Keyword(s):  
Biological Fluids ◽  
Direct Determination ◽  
Differential Pulse ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Electrochemical Parameters ◽  
Standard Rate ◽  
Voltammetric Methods ◽  
Standard Rate Constant

Electrochemical behavior of atorvastatin (AT) and optimum conditions to its quantitative determination were investigated using voltammetric methods. Some electrochemical parameters such as diffusion coefficient, surface coverage of adsorbed molecules, electron transfer coefficient, standard rate constant and number of electrons were calculated using the results of cyclic voltammetry. A tentative mechanism for the oxidation for AT has been suggested. The oxidation signal of AT molecule was used to develop fully validated, new, rapid, selective and simple square-wave anodic adsorptive stripping voltammetric (AdsSWV) and differential pulse anodic stripping voltammetric (AdsDPV) methods to direct determination of AT in pharmaceutical dosage forms and biological samples. For the AdsDPV and AdsSWV techniques, linear working ranges were found to be 1.0 × 10–7–5.0 × 10–6and 3.0 × 10–7–5.0 × 10–6mol l–1, respectively. The detection limits obtained from AdsDPV and AdsSWV were calculated to be 6.55 × 10–8and 1.53 × 10–7mol l–1, respectively. The methods were successfully applied to assay the drug in tablets, human blood serum and human urine.

Square-wave cathodic adsorptive stripping voltammetry of risperidone

2011 ◽  
Vol 76 (3) ◽  
pp. 159-176 ◽  
Author(s):  
Ibrahim Hüdai Taşdemir ◽  
Orhan Çakirer ◽  
Nevin Erk ◽  
Esma Kiliç
Keyword(s):  
Human Serum ◽  
Human Urine ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Reduction Wave ◽  
Pharmaceutical Dosage Forms ◽  
Peak Current ◽  
Square Wave ◽  
Relative Standard ◽  
Spiked Human Urine

Electrochemical properties and diffusion-adsorption behavior of risperidone (RPN), an antiphyscotic drug, on hanging mercury drop electrode (HMDE) were carried out in Britton–Robinson (BR) buffer. Some electrochemical parameters such as diffusion coefficient, number of transferred electrons and proton participated to its reduction mechanism and surface coverage coefficient were calculated from the results of cyclic voltammetry, square-wave voltammetry and constant potential electrolysis. RPN was found to be reduced with single two-electron/two-proton quasi-reversible mechanism controlled mainly by adsorption with some diffusion contribution at the potential about –1.58 V (vs Ag|AgCl electrode). Experimental parameters were optimized to develop a new, accurate, rapid, selective and simple square-wave cathodic adsorptive stripping voltammetric (SWCAdSV) method for direct determination of RPN in pharmaceutical dosage forms, spiked human urine and human serum samples without time-consuming steps prior to drug assay. This method was based on the relation between the peak current and the concentration of RPN and it was recognized that peak current of reduction wave linearly changes with the concentration of RPN in the concentration range of 1.5–150 nM, when optimum preconcentration potential –0.65 V and optimum preconcentration time 60 s were applied. In this method, limit of detection (LOD) was found as 5.18 nM (2.12 ppb). The method was successfully applied to determine the RPN content of commercial pharmaceutical preparations, spiked human serum and spiked human urine. The method was found to be highly accurate and precise, having a relative standard deviation of less than 4.80% for all applications.

scholarly journals DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC METHOD FOR QUANTITATIVE ESTIMATION OF LAFUTIDINE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (6) ◽  
pp. 75
Author(s):  
Ritesh Kumar ◽  
Amrish Chandra ◽  
Swati Gupta ◽  
Pawan Kumar Gautam
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Ultra Violet ◽  
Dosage Forms ◽  
Uv Absorption ◽  
Uv Spectrophotometry ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms

Objective: The objectives of the present research was to develop a simple, precise, economical, accurate, reproducible and sensitive method for the quantitative estimation of lafutidine in bulk and its pharmaceutical dosage forms by Ultra Violet (UV) absorption spectrophotometry.Methods: The method uses 0.1 N HCl, pH 1.20 as a solvent of choice for the quantitative estimation of lafutidine in bulk and its tablets dosage form by UV absorption spectrophotometry at a wavelength of 290 nm. The method was validated for parameters like linearity, range, precision, Limit of Detection (LOD), Limit of Quantification (LOQ), accuracy, recovery and stability of the analyte.Results: Lafutidine exhibited absorbance maxima at 290 nm in 0.1 N HCl, pH 1.20 solvent. The developed method was validated as per the ICH validation guidelines. Beer’s law was obeyed in range of 0-30 µg/ml with r2= 0.9997. The LOD and LOQ values of lafutidine were found to be 0.545 µg/ml and 1.654 µg/ml respectively. The mean % recovery for the developed method was found to be in the range of 99.25 to 99.45 % respectively for the marketed dosage forms. The developed method was also found to be robust.Conclusion: The developed method was found suitable for the routine quantitative analysis of lafutidinein bulk and pharmaceutical dosage form. It was also concluded that developed UV spectrophotometry method was accurate, precise, linear, reproducible, robust and sensitive.

RP-HPLC Assay for Estimation of Pitavastatin in Bulk and Pharmaceutical Dosage Forms

2014 ◽  
Vol 7 (1) ◽  
pp. 2346-2349
Author(s):  
K Tirumala ◽  
CH.V.S Gautam ◽  
J Gangadhar ◽  
M Jayajeevitha ◽  
Vanitha Prakash K
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Bulk Drug

Reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the estimation of pitavastatin in tablet dosage form. A Phenomenex Luna C18, 150×4.6 mm i.d, 5 µm particle size with mobile phase consisting of buffer 0.01M potassium dihydrogen ortho phosphate pH (3.75) adjusted with dilute orthophosphoric and acetonitrile in the ratio of 20:80 v/v was used. The flow rate was 1.2 mL/min and eluents were monitored at 248 nm. The retention time was 4.1min. The detector response was linear in the concentration of 25-150 µg/mL, with the regression coefficient of 0.9998. Quantification was done by calculating area of the peak and the limit of detection and limit of quantification were 1.9 µg/mL and 5.7 µg/mL respectively. The percentage assay of pitavastatin was 101.1%. The results of study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate which is useful for the routine determination of pitavastatin in bulk drug and in its pharmaceutical dosage forms.

HPTLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF CHLORTHALIDONE AND IRBESARTAN IN COMBINED TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (07) ◽  
pp. 46-52
Author(s):  
P Kalaiselvi ◽  
◽  
K. G. Lalitha
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Ammonia Solution ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Tablet Dosage ◽  
Hptlc Method

A simple, accurate and rapid high performance thin layer chromatography (HPTLC)-densitometry method was developed for separation and determination of chlorthalidone (CHL) and irbesartan (IBS) in pharmaceutical dosage forms. The compounds were separated on silica gel 60 GF254, HPTLC plates using mobile phase of toluene: ethyl acetate: acetonitrile: methanol: ammonia solution (25%) [5:2:2:1:0.2 v/v/v/v] as compact spots at Rf of 0.57 for chlorthalidone and Rf of 0.36 for irbesartan. Densitometric detection was performed at 254 nm. The method was validated in terms of linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ). The calibration curves were linear in the range of 12.5-75 ng/spot for CHL and 150-900ng/spot for IBS. For CHL recovery varied in range of 99.26-101.25% and for IBS recovery varied in range of 99.76-100.40%. The LOD was found 1.33 and 11.34 ng/spot for CHL and IBS respectively. The LOQ was found 4.03 and 14.37 ng /spot for CHL and IBS respectively. It was observed that the proposed HPTLC method could be used for efficient analysis of the CHL and IBS in combined tablet dosage forms.

scholarly journals Spectrophotometric Method for the Determination of Drugs Containing Phenol Group by Using 2, 4- Dinitrophenylhydrazine

2010 ◽  
Vol 7 (2) ◽  
pp. 395-402
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Kumar Shrestha
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Phenolic Drugs

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.

DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF FENSPIRIDE HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORMS.

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (01) ◽  
pp. 20-25
Author(s):  
S. M Samyuktha ◽  
◽  
P. G Prasanthi ◽  
K Mahesh ◽  
B. N Nalluri ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, accurate High Performance Liquid Chromatographic (HPLC) method was developed and validated for the analysis of Fenspiride hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved isocratically using a C18 reverse phase column [Inertsil C18 column (250×4.6mm, 5μm)] utilizing a mobile phase containing 10mM Ammonium acetate: Acetonitrile (50:50 v/v) at a flow rate of 1 mL/min. The eluents were monitored at wavelength of 210 nm for a run time of 7 minutes at ambient temperature. The average retention time of the drug was found to be 4.6 minutes. The developed method was validated as per ICH guidelines to ascertain the reproducibility of the method. The method was found to be linear in the concentration range of 10-50 μg/mL with a good correlation coefficient of 0.998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.007 and 0.021 μg/mL and the percentage recovery and assay were found to be 99.315 and 98.97%. Specificity with placebo by 3 D plots showed that the method was specific and free from interfering substances. Therefore, the fully validated method was good enough to carry out routine analysis of Fenspiride in bulk and tablet formulations.

scholarly journals Validation and Application of a Modified RP-HPLC Method for the Quantification of Desloratadine in Pharmaceutical Dosage Forms

1970 ◽  
Vol 5 (1) ◽  
pp. 1-4 ◽  
Author(s):  
BM Mahbubul Alam Razib ◽  
Md. Ashik Ullah ◽  
Mohammad Abdul Kalam Azad ◽  
Rebeka Sultana ◽  
Hasina Yasmin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Acid Sodium Salt

The purpose of the study was to develop a simple, sensitive and rapid RP-HPLC method for the determination of desloratadine in marketed products. Chromatographic determination was performed in a reverse phase C18 column (250 mm × 3.3 mm I.D. , 5?m particle size) using a mixture of acetonitrile ? n-pentane sulphonic acid sodium salt monohydrate, adjusted to pH 3.0± 0.05 with phosphoric acid (60? 40 v/v) as mobile phase and delivered at a flow rate of 1 ml/min. The UV detection was set at 254 nm. The calibration range was from 2.0 to 40 ?g/ml. The method was validated in term of linearity (r2>0.98, RSD= 1.958%), precision (RSD=3.757 %) and accuracy (deviation>2.653%, RSD> 2.203%). The limit of quantification was 2 ?g/ml and the limit of detection was 0.1 ?g/ml. The linear ranges of desloratadine were 20.23 ± 0.368 ?g/ml and 6.545 ± 0.0495 ?g/ml in tablet (potency = 99.175 ± 0.718 %) and syrup (potency = 101.15 ± 1.838 %) respectively. The potency of desloratadine in marketed products was determined by this method with acceptable precision and reproducibility. Keywords: Desloratadine, marketed products, RP-HPLC, development of a method Dhaka Univ. J. Pharm. Sci. Vol.5(1-2) 2006 The full text is of this article is available at the Dhaka Univ. J. Pharm. Sci. website

Quantitative Nuclear Magnetic Resonance Spectroscopic Analysis of Two Commonly Used Gastrointestinal Tract Drugs

2020 ◽  
Vol 103 (5) ◽  
pp. 1208-1214
Author(s):  
Ramzia I Elbagary ◽  
Marwa A Fouad ◽  
Menna I Ezzeldin
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Quantitative Monitoring ◽  
Quantitative Nuclear Magnetic Resonance ◽  
Nuclear Magnetic

Background Two fast and precise quantitative nuclear magnetic resonance spectroscopic methods (qNMR) were established and evaluated for the determination of ondansetron (OND) and omeprazole (OMP) in bulk drugs and their pharmaceutical dosage forms. NMR spectra were established using dimethylsulfoxide (DMSO-d6) as a solvent and phloroglucinol as the internal standard. Proton NMR signals at 3.743, 3.811, and 5.670 ppm were used for quantitative monitoring purposes corresponding to OND, OMP, and phloroglucinol, respectively. In this study, the methods linearity, accuracy, limit of quantification, limit of detection, stability, and precision were validated as per International Conference on Harmonization (ICH) guidelines. Linearity ranges were 0.3–10 mg for OND and 1–10 mg for OMP. The student t-test and F-test were used for statistical evaluation. Herein, the proposed methods are useful and can be a successful practical appliance for OND and OMP determination in drug substances and their dosage forms.

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