scholarly journals Different Spectrophotometric Methods for Simultaneous Determination of Trelagliptin and Its Acid Degradation Product

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Shereen Mowaka ◽  
Bassam M. Ayoub ◽  
Mostafa A. Hassan ◽  
Wafaa A. Zaghary
Keyword(s):  
Degradation Product ◽  
Simultaneous Equation ◽  
Chemometric Methods ◽  
Acid Degradation ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Mean Centering ◽  
Validation Parameters ◽  
Major Acid

New spectrophotometric and chemometric methods were carried out for the simultaneous assay of trelagliptin (TRG) and its acid degradation product (TAD) and applied successfully as a stability indicating assay to recently approved Zafatek® tablets. TAD was monitored using TLC to ensure complete degradation. Furthermore, HPLC was used to confirm dealing with one major acid degradation product. The proposed methods were developed by manipulating zero-order, first-derivative, and ratio spectra of TRG and TAD using simultaneous equation, first-derivative, and mean-centering methods, respectively. Using Spectra Manager II and Minitab v.14 software, the absorbance at 274 nm–260.4 nm, amplitudes at 260.4 nm–274.0 nm, and mean-centered values at 287.6 nm–257.2 nm were measured against methanol as a blank for TRG and TAD, respectively. Linearity and the other validation parameters were acceptable at concentration ranges of 5–50 μg/mL and 2.5–25 μg/mL for TRG and TAD, respectively. Using one-way analysis of variance (ANOVA), the optimized methods were compared and proved to be accurate for the simultaneous assay of TRG and TAD.

Validated Stability-Indicating Spectrophotometric Methods for the Determination of Cefixime Trihydrate in the Presence of its Acid and Alkali Degradation Products

2015 ◽  
Vol 98 (1) ◽  
pp. 35-45 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Regression Equations ◽  
Acid Degradation ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Accuracy And Precision ◽  
Significant Difference

Abstract Five simple, accurate, precise, and economical spectrophotometric methods have been developed for thedetermination of cefixime trihydrate (CFX) in the presence of its acid and alkali degradation products without prior separation. In the first method, secondderivative (2D) and first derivative (1D) spectrophotometry was applied to the absorption spectra of CFX and its acid (2D) or alkali (1D) degradation products by measuring the amplitude at 289 and 308 nm, respectively. The second method was a first derivative (1DD) ratio spectrophotometric method where the peak amplitudes were measured at 311 nm in presence of the acid degradation product, and 273 and 306 nm in presence of its alkali degradation product. The third method was ratio subtraction spectrophotometry where the drug is determined at 286 nm in laboratory-prepared mixtures of CFX and its acid or alkali degradation product. The fourth method was based on dualwavelength analysis; two wavelengths were selected at which the absorbances of one component were the same, so wavelengths 209 and 252 nm were used to determine CFX in presence of its acid degradation productand 310 and 321 nm in presence of its alkali degradation product. The fifth method was bivariate spectrophotometric calibration based on four linear regression equations obtained at the wavelengths 231 and 290 nm, and 231 and 285 nm for the binary mixture of CFX with either its acid or alkali degradation product, respectively. The developed methods were successfully applied to the analysis of CFX in laboratory-prepared mixtures and pharmaceutical formulations with good recoveries, and their validation was carried out following the International Conference on Harmonization guidelines. The results obtained were statistically compared with each other and showed no significant difference with respect to accuracy and precision.

scholarly journals Three Different Spectrophotometric Methods for Simultaneous Determination of Pyriproxyfen and Chlorothalonil Residues in Cucumber and Cabbage Samples

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre
Keyword(s):  
Simultaneous Determination ◽  
Simultaneous Estimation ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
The Third ◽  
Mean Centering ◽  
Relative Standard ◽  
One Way Anova

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.

scholarly journals Comparative Study of Novel Ratio Spectra and Isoabsorptive Point Based Spectrophotometric Methods: Application on a Binary Mixture of Ascorbic Acid and Rutin

2016 ◽  
Vol 2016 ◽  
pp. 1-12
Author(s):  
Hany W. Darwish ◽  
Ahmed H. Bakheit ◽  
Ibrahim A. Naguib
Keyword(s):  
Ascorbic Acid ◽  
Binary Mixture ◽  
High Performance ◽  
Pharmaceutical Tablets ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ratio Difference ◽  
Mean Centering ◽  
Assay Conditions

This paper presents novel methods for spectrophotometric determination of ascorbic acid (AA) in presence of rutin (RU) (coformulated drug) in their combined pharmaceutical formulation. The seven methods are ratio difference (RD), isoabsorptive_RD (Iso_RD), amplitude summation (A_Sum), isoabsorptive point, first derivative of the ratio spectra (1DD), mean centering (MCN), and ratio subtraction (RS). On the other hand, RU was determined directly by measuring the absorbance at 358 nm in addition to the two novel Iso_RD and A_Sum methods. The work introduced in this paper aims to compare these different methods, showing the advantages for each and making a comparison of analysis results. The calibration curve is linear over the concentration range of 4–50 μg/mL for AA and RU. The results show the high performance of proposed methods for the analysis of the binary mixture. The optimum assay conditions were established and the proposed methods were successfully applied for the assay of the two drugs in laboratory prepared mixtures and combined pharmaceutical tablets with excellent recoveries. No interference was observed from common pharmaceutical additives.

Development and Validation of Spectrophotometric Methods for the Determination of Canagliflozin or Gliclazide and Metformin in the Presence of Metformin Impurity (1-Cyanoguanidine)

2019 ◽  
Vol 102 (4) ◽  
pp. 1112-1124
Author(s):  
Sonia T Hassib ◽  
Elham A Taha ◽  
Ehab F Elkady ◽  
Ghada H Barakat
Keyword(s):  
Second Step ◽  
Chemometric Methods ◽  
Chemometric Method ◽  
Spectrophotometric Methods ◽  
Enrichment Technique ◽  
Validation Parameters ◽  
Sample Enrichment ◽  
Development And Validation ◽  
Separation Results

Abstract Background: Quantitative multicomponent analysis is considered an analytical goal to save time and cost in analysis. Objective: This work aimed to provide sensitive and selective [successive ratio subtraction coupled with constant multiplication (SRS-CM) and chemometric] methods for the determination of coformulated antidiabetic drugs, namely canagliflozine and metformin or gliclazide and metformin in presence of metformin degradation product, 1-cyanoguanidine. Methods: SRS-CM method was developed for the determination of canagliflozin and metformin at 292 and 237 nm, respectively, using 14 μg/mL canagliflozin as a divisor in the first step to cancel the spectrum of canagliflozin. Then, 18 μg/mL metformin was used as a divisor in the second step to cancel the spectrum of metformin. Finally, we obtained the spectrum of cyanoguanidine. Chemometric method was applied for the determination of the gliclazide and metformin mixture in a 225–235 nm range. Sample enrichment technique was used to increase the concentration of canagliflozin or gliclazide to allow its simultaneous determination with metformin without prior separation. Results: Validation parameters according to the International Conference on Harmonization guidelines were satisfactory over the concentration ranges of 5 to 16 μg/mL for canagliflozin and metformin as well as 2.5 to 12.5 and 6 to 24 μg/mL for gliclazide and metformin, respectively. Conclusions: The method provides sufficient selectivity and accuracy to be applied for routine analysis and quality control in laboratories for the cited drugs. Highlights: This work shows two examples to how to select a suitable UV spectrophotometric method to overcome the spectral overlap.

Eco-friendly spectrophotometric methods for assessment of alfuzosin and solifenacin in their new pharmaceutical formulation; Green profile evaluation via eco-scale and GAPI tools

2020 ◽  
Vol 16 ◽  
Author(s):  
Mamdouh R. Rezk ◽  
Mina Wadie ◽  
Soheir A. Weshahy ◽  
Mahmoud A. Tantawy
Keyword(s):  
Minor Component ◽  
Time Saving ◽  
Prostate Hyperplasia ◽  
Spectrophotometric Methods ◽  
Ratio Difference ◽  
Ich Guidelines ◽  
Mean Centering ◽  
Benign Prostate ◽  
Urological Diseases

Background: Alfuzosin is recently co-formulated with solifenacin for relieving two coincident urological diseases, namely; benign prostate hyperplasia and overactive bladder Objective: Herein, green, simple and rapid spectrophotometric methods were firstly developed for simultaneous determination of the two cited drugs in their co-formulated pharmaceutical capsule Methods: Alfuzosin, which is the major component in the dosage form, was directly assayed at its extended wavelength at 330.0 nm. The challenging spectrum of the minor component, solifenacin, was resolved by five spectrophotometric methods, namely; dual wavelength (DW) at 210.0 & 230.0 nm, first derivative (1D) at 222.0 nm, ratio difference (RD) at 217.0 - 271.0 nm , derivative ratio (1DD) at 223.0 and mean centering of ratio spectra (MC) at 217.0 nm Results: The Proposed methods were successfully validated as per ICH guidelines. Alfuzosin showed linearity over the range of 4.0 - 70.0 μg/mL, while that of solifenacin were 4.0 - 50.0 μg/mL for DW, 2.0 - 70.0 μg/mL for 1D and RD methods, 1.0 - 70.0 μg/mL for 1DD and 4.0 - 70.0 μg/mL for MC method. Statistical comparison with their official ones showed no noticeable differences. The methods showed good applicability for assaying drugs in their newly combination. Besides eco-scale, the greenness profile of the methods was assessed and compared with the reported spectrophotometric one via the newest metric tool; green analytical procedure index (GAPI). Conclusions: The proposed methods are superior in not only being smart, accurate, selective, robust and time-saving, but also in using distilled water as an eco-friendly and cheap solvent

scholarly journals Simultaneous Estimation of Domperidone and Pantoprazole in Solid Dosage Form by UV Spectrophotometry

2006 ◽  
Vol 3 (3) ◽  
pp. 142-145
Author(s):  
P. Ravi Kumar ◽  
P. Bhanu Prakash ◽  
M. Murali Krishna ◽  
M. Santha Yadav ◽  
C. Asha Deepthi
Keyword(s):  
Simultaneous Equation ◽  
Simultaneous Equations ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Q Value ◽  
Value Analysis ◽  
Spectrophotometric Methods ◽  
Solid Dosage ◽  
Tablet Dosage

Domperidone is an antiemetic and pantoprazole is an antiulcer drug. Simple, precise, rapid and selective simultaneous equation and Q- analysis UV spectrophotometric methods have been developed for the simultaneous determination of domperidone and pantoprazole from combined tablet dosage forms. The methods involve solving of simultaneous equations and Q-value analysis based on measurement absorptivity at 216, 287 and 290 nm respectively. Linearity lies between 1-15 mcg/mL for domperidone and 0-50 mcg/mL for pantoprazole.

scholarly journals Synchronous fluorescence as a green and selective tool for simultaneous determination of bambuterol and its main degradation product, terbutaline

2018 ◽  
Vol 5 (10) ◽  
pp. 181359 ◽  
Author(s):  
Samah Abo El Abass ◽  
Heba Elmansi
Keyword(s):  
Degradation Product ◽  
Low Cost ◽  
Reference Method ◽  
Cost Effective ◽  
Zero Crossing ◽  
Cost Effective Method ◽  
Validation Parameters ◽  
Main Degradation Product ◽  
20 Nm

A green, sensitive and cost-effective method is introduced in this research for the determination of bambuterol and its main degradation product, terbutaline, simultaneously, relying on the synchronous spectrofluorimetric technique. First derivative synchronous spectrofluorimetric amplitude is measured at Δ λ = 20 nm, so bambuterol can be quantitated at 260 nm, and terbutaline can be measured at 290 nm, each at the zero crossing point of the other. The amplitude–concentration plots were linear over the concentration ranges of 0.2–6.0 µg ml −1 and 0.2–4.0 µg ml −1 for both bambuterol and terbutaline, respectively. Official guidelines were followed to calculate the validation parameters of the proposed method. The low values of limits of detection of 0.023, 0.056 µg ml −1 and limits of quantitation of 0.071, 0.169 µg ml −1 for bambuterol and terbutaline, respectively, point to the sensitivity of the method. Bambuterol is a prodrug for terbutaline, and the latter is considered its degradation product so the established method could be regarded as a stability-indicating one. Moreover, the proposed method was used for the analysis of bambuterol and terbutaline in their single ingredient preparations and the results revealed statistical agreement with the reference method. The suggested method, being a simple and low-cost procedure, is superior to the previously published methods which need more sophisticated techniques, longer analysis time and highly toxic solvents and reagents. It could be considered as an eco-friendly analytical procedure.

DC Polarographic and Spectrophotometric Determination of Ampicillin Capsules

1980 ◽  
Vol 63 (5) ◽  
pp. 1049-1051
Author(s):  
Juan A Squella ◽  
Luis J Nunez-Vergara ◽  
Maximo Aros
Keyword(s):  
Absorption Band ◽  
Spectrophotometric Determination ◽  
Degradation Product ◽  
Uv Absorption ◽  
Acidic Hydrolysis ◽  
Average Recovery ◽  
Polarographic Wave ◽  
Spectrophotometric Methods ◽  
Hydrolysis Of

Abstract Polarographic and spectrophotometric methods are proposed for the determination of ampicillin in capsules. Acidic hydrolysis of ampicillin with 1% HCHO in 0.3N HCl yields a degradation product identified as 2-hydroxy-3-phenyl-6-methylpyrazine. This compound has a well defined UV absorption band at 380 nm and a polarographic wave at –0.55 V vs SCE, which can be used for analytical purposes. Individual capsule assays, composite assays, and recovery studies are described. The average recovery values and standard deviations (SD) for UV and polarographic determinations were 99.20% (SD 0.95) and 100.85% (SD 1.09), respectively

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