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.

scholarly journals HPLC, Densitometric and Spectrophotometric Methods for the Simultaneous Determination of Colchicine and Probenecid in Their Binary Mixture

2019 ◽  
pp. 1-12 ◽  
Author(s):  
Samah Abd Elsabour Mohammed ◽  
Sawsan Abd El Moneim Abd El-Razeq ◽  
Israa Abd Elgafar Mohammed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Binary Mixture ◽  
Mobile Phase ◽  
High Performance ◽  
Zero Order ◽  
Spectrophotometric Methods ◽  
Ratio Difference ◽  
Mean Centering

Aim: To develop methods with  complete validation according to ICH guidelines and to be  applied for the determination of both drugs in laboratory prepared mixtures and in pharmaceutical formulation Study Design: High performance liquid chromatography (HPLC), densitometric and different spectrophotometric methods (zero order, derivative ratio, ratio difference and mean centering) are developed for simultaneous determination of colchicine and probenecid in their combined pharmaceutical formulation.  Methodology: High performance liquid chromatography separation is developed using C18 column and methanol: ammonia (100: 1.5 v/v) as a mobile phase. The densitometric method based on the separation of both drugs using chloroform: methanol: ethyl acetate: water: ammonia (7: 5:2.5:0.5:0.5 by volume) as mobile phase and scanning λ at 254 nm. Zero order determination is based on measurement of colchicine absorbance at 349 nm.  The first derivative ratio of peak amplitudes at 367 nm& at 290.4 nm and the ratio difference with the amplitude difference between (385 nm and 362.4 nm) and ( 270 nm and 255 nm)  for colchicine and probenecid, respectively are developed for the determination of both drugs. Mean centering determination of probenecid is developed by measurement at 279 nm using 3.6 µg/mL of colchicine as a divisor. Results: HPLC method was applied over the  concentration ranges of 1.0-45.0 µg/mL & 0.5-30.0, while densitometric method was  linear over the concentration 0.15. 0-0.6 & 0.15-0.45 µg / band  and spectrophotometric methods were linear over the concentration ranges 10.00-55.0 & 3.6-20.0 µg/mL  for colchicine and probenecid, respectively. Conclusion: Novel, simple and accurate method for the determination of colchicine and probenecid simultaneously in their binary mixture.

scholarly journals Validated Stability Indicating HPTLC, UHPLC and UV-Spectrophotometric Techniques for the Determination of Bepotastine Besilate in Presence of Its Oxidative Degradate

2019 ◽  
pp. 1-14 ◽  
Author(s):  
Marwa Mohammed Soliman ◽  
Manal Kamal Darwish ◽  
Sawsan Abdel-Moneem Abdel-Razeq
Keyword(s):  
High Performance ◽  
Oxidative Degradation ◽  
Pharmaceutical Formulations ◽  
Stability Indicating ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ratio Difference ◽  
Ich Guidelines ◽  
Developing System

The study is aimed at developing methods which have a complete validation as stipulated in the ICH guidelines and to be applied for the determination of Bepotastine besilate (BB) in pure form and in pharmaceutical formulations in the presence of its oxidative degradation product. High performance thin layer chromatography (HPTLC), Ultra high performance liquid chromatography (UHPLC) and different spectrophotometric methods (first derivative, first derivative of ratio spectra and ratio difference are developed for simultaneous determination of bepotastine besilate in laboratory-prepared mixtures of bepotastine besilate with its oxidative degradate and in pharmaceutical formulations were used in the study design. Firstly, HPTLC was performed and separation occurred on silica gel 60 F254 plates, with butanol: ammonia (8:2, v/v) as a developing system. UHPLC in which separation occurred on a Kinetex C 18 column using methanol- 0.1% O-phosphoric acid - acetonitrile (70:20:10, by volume) as mobile phase, followed. And lastly was UV/Vis spectrophotometry which included first derivative determination of the drug at 252.6 nm, first derivative of ratio of peak amplitudes at 233.4, 250 and 275.6 nm and the ratio difference with the amplitude difference between (240 nm and 260 nm). Result showed that HPTLC method was applicable over the concentration range of 0.5-5 μg / band, while UHPLC method was linear over the concentration 2- 12 μg/mL and spectrophotometric methods were linear over the concentration range 20-120 μg/mL for bepotastine besilate. The proposed three techniques are quite accurate and precise. They can be used for routine analysis of bepotastine besilate in pharmaceutical formulation and stability indicating methods.

scholarly journals Validated Stability Indicating HPTLC and UV-Spectrophotometric Techniques for the Determination of Avanafil

2019 ◽  
pp. 1-16 ◽  
Author(s):  
Manal K. Darwish ◽  
Marwa M. Soliman ◽  
Sawsan A. Abdel-Razeq
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Accurate Method ◽  
Pharmaceutical Formulation ◽  
Dual Wavelength ◽  
Uv Spectrophotometry ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ratio Difference

Aims: To develop methods with complete validation according to ICH guidelines and to be applied for the determination of avanafil in pure form and in pharmaceutical formulation in the presence of its degradation products. Study Design: High performance thin layer chromatography (HPTLC) and different spectrophotometric methods (dual wavelength, first derivative, first derivative of ratio spectra and ratio difference are developed for simultaneous determination of avanafil in laboratory-prepared mixtures of avanafil with its degradation products and in pharmaceutical formulation. Place and Duration of Study: Sample: Department of Analytical Chemistry, Faculty of Pharmacy (Girls), Al-Azhar University, Cairo, Egypt, between May 2019 and September 2019. Methodology: Two techniques have been developed for the determination of avanafil in the presence of its degradation products. The first was HPTLC where separation was performed on silica gel 60 F254 plates, with chloroform: toluene: methanol: conc. ammonia (6:5:3:0.1, by volume) as a developing system and UV detection at 230 nm. The second one was UV- spectrophotometry which included dual wavelength between 267 and 292 nm, first derivative determination of the drug at 261 nm, first derivative of ratio of peak amplitudes at 275.6, 305.4 and 329 nm and the ratio difference with the amplitude difference between (266 and 250 nm). Results: HPTLC method was applied over the concentration range of 0.5-5. μg/spot, while spectrophotometric methods were linear over the concentration range 5-50 μg/mL for avanafil. Conclusion: Novel, simple and accurate method for the determination of avanafil in laboratory-prepared mixtures of avanafil with its degradation products and in pharmaceutical formulation.

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 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 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.

scholarly journals Determination of Metformin Hydrochloride and Glyburide in an Antihyperglycemic Binary Mixture Using High-Performance Liquid Chromatographic-UV and Spectrometric Methods

2010 ◽  
Vol 93 (1) ◽  
pp. 133-140 ◽  
Author(s):  
Hesham Salem
Keyword(s):  
Binary Mixture ◽  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Metformin Hydrochloride ◽  
Second Derivative ◽  
Zero Crossing ◽  
First Derivative

Abstract Three methods were developed for simultaneous determination of metformin hydrochloride and glyburide in an antihyperglycemic binary mixture without previous separation. In the first method, a reversed-phase HPLC column with acetonitrilewater (60 + 40, v/v) mobile phase at 0.9 mL/min flow rate was used to separate both compounds, with UV detection at 254 nm. Linearity was obtained in the concentration range of 0.060.24 µg/mL for glyburide and 1.56.0 µg/mL for metformin hydrochloride. The second method depended on first- and second-derivative UV spectrometry with zero-crossing measurements. The first-derivative amplitude at 261 nm was selected for the assay of glyburide, and the second-derivative amplitude at 235 nm was selected for the assay of metformin hydrochloride. The third method depended on measuring the first derivative of the ratio-spectra at 241 nm for glyburide and 227 nm for metformin hydrochloride. For the second and third methods, Beer's law was obeyed in the range of 1055 µg/mL for glyburide and 20200 µg/mL for metformin. The proposed methods were extensively validated and applied for the analysis of some pharmaceutical formulations containing binary mixtures of the mentioned drugs.

scholarly journals Simultaneous Determination of Moxifloxacin and Flavoxate by RP-HPLC and Ecofriendly Derivative Spectrophotometry Methods in Formulations

2019 ◽  
Vol 16 (7) ◽  
pp. 1196 ◽  
Author(s):  
Mahesh Attimarad ◽  
Muhammad Shahzad Chohan ◽  
Abdulmalek Ahmed Balgoname
Keyword(s):  
Simultaneous Determination ◽  
Spectrophotometric Method ◽  
High Performance ◽  
Internal Standard ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
First Derivative

Simple, fast, and precise reversed-phase (RP)-high-performance liquid chromatography (HPLC) and two ecofriendly spectrophotometric methods were established and validated for the simultaneous determination of moxifloxacin HCl (MOX) and flavoxate HCl (FLX) in formulations. Chromatographic methods involve the separation of two analytes using an Agilent Zorbax SB C18 HPLC column (150 mm × 4.6 mm; 5 µm) and a mobile phase consisting of phosphate buffer (50 mM; pH 5): methanol: acetonitrile in a proportion of 50:20:30 v/v, respectively. Valsartan was used as an internal standard. Analytes were monitored by measuring the absorbance of elute at 299 nm for MOX and 250 nm for FLX and valsartan. Two environmentally friendly spectrophotometric (first derivative and ratio first derivative) methods were also developed using water as a solvent. For the derivative spectrophotometric determination of MOX and FLX, a zero-crossing technique was adopted. The wavelengths selected for MOX and FLX were −304.0 nm and −331.8 nm for the first derivative spectrophotometric method and 358.4 nm and −334.1 nm for the ratio first-derivative spectrophotometric method, respectively. All methods were successfully validated, as per the International Conference on Harmonization(ICH) guidelines, and all parameters were well within acceptable ranges. The proposed analytical methods were successfully utilized for the simultaneous estimation of MOX and FLX in formulations.

scholarly journals Development and Validation of Column High-Performance Liquid Chromatographic and Derivative Spectrophotometric Methods for Determination of Levofloxacin and Ornidazole in Combined Dosage Forms

2008 ◽  
Vol 91 (4) ◽  
pp. 756-761 ◽  
Author(s):  
Satish A Patel ◽  
Arun M Prajapati ◽  
Paresh U Patel ◽  
Natubhai J Patel ◽  
Jayesh B Vaghmasi
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Rp Hplc ◽  
Liquid Chromatographic

Abstract The manuscript describes validated reversed-phase column high-performance liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of levofloxacin (LFX) and ornidazole (ORNI) in combined dosage forms. The RP-HPLC separation was achieved on a Phenomenex C18 column (250 mm 4.6 mm id, 5 m) using KH2PO4 buffer (pH 6.8)methanolacetonitrile (70 + 15 + 15, v/v/v) mobile phase at a flow rate of 1.5 mL/min and ambient temperature (25 2<sup/>C). Quantification was achieved with photodiode array detection at 295 nm over the concentration range of 110 g/mL for both LFX and ORNI, with mean recovery of 101.7 0.23 and 99.23 1.57, respectively, by the RP-HPLC method. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first-order derivative spectra were obtained at N =1 (scaling factor), = 2.0 nm (wavelength interval), and the determinations were made at 310 nm (ZCP of ORNI) for LFX and 295 nm (ZCP of LFX) for ORNI over the concentration range of 240 g/mL for both LFX and ORNI. Mean recovery was 99.46 0.96 and 100.9 0.72, respectively, by the first-derivative UV spectrophotometric method. Standard and sample solutions were prepared with methanol as the solvent in both of the methods. These methods were found to be simple, accurate, precise, and sensitive and were applicable for the simultaneous determination of LFX and ORNI in combined dosage forms.

scholarly journals Simultaneous Kinetic Spectrophotometric Determination Of Ascorbic Acid And Cysteine With An Optical Probe By Mean Centering Of Ratio Kinetic Profiles Method

2019 ◽  
Vol 14 (3) ◽  
pp. 163-170
Author(s):  
A.B. Vishnikin ◽  
Yu.V. Miekh ◽  
Ya.R. Bazel ◽  
M.E.A. Al-Shwaiyat ◽  
G.O. Petrushina
Keyword(s):  
Ascorbic Acid ◽  
Binary Mixture ◽  
Standard Addition ◽  
Optical Probe ◽  
Addition Method ◽  
Kinetic Measurements ◽  
Mean Centering ◽  
The Difference ◽  
Kinetic Spectrophotometric

A procedure for simultaneous kinetic analysis of a binary mixture of ascorbic acid (Asc) and cysteine (Cys) was developed using the method of mean centering of ratio kinetic profiles. The method is based on the difference in the rate of reactions of Asc and Cys with the complex of iron(III) with o-phenanthroline at pH 7.05. The use of an optical probe simplifies the carrying out of kinetic measurements, allows to obtain highly reproducible (Sr=0.01-0.02) results, and significantly reduces the time of analysis. The method of mean centering of ratio kinetic profiles is superior to the H-Point standard addition method, since it does not require such a long measurement time and there is no restriction on the constancy of absorbance of one of the components. Asc and Cys can be determined in the concentration range from 1 to 10 mg/L. The method was successfully used to determine Asc and Cys in dietary supplements.

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