A Smart Green Spectrophotometric Method for Simultaneous Determination of Severely Overlapped Binary Mixtures Using Normalized Spectrum and Isosbestic Point as Resolving Tools

2020 ◽  
Vol 16 (3) ◽  
pp. 254-261
Author(s):  
Ekram H. Mohamed ◽  
Ahmed Hamza ◽  
Aya Reda ◽  
Ola Adel ◽  
Sara Atef
Keyword(s):  
Binary Mixture ◽  
Simultaneous Determination ◽  
Total Concentration ◽  
Accurate Method ◽  
Ternary Mixtures ◽  
Isosbestic Point ◽  
First Derivative ◽  
Ich Guidelines

Background: The ability of the normalized spectra when used as a divisor and in combination with isosbestic point to resolve complex binary or ternary mixtures, Candesartan and Hydrochlorthiazide binary mixture was taken as a model. Introduction: A green simple smart and accurate method using ethanol as a solvent namely simultaneous derivative ratio (SIDD) was applied to prove the power of normalized spectra and isosbestic point as spectrophotometric resolving tools. Methods: In the proposed SIDD method, the zero order spectra of drugs were simply manipulated using the normalized spectra of CAN as divisor to obtain the ratio and first derivative spectra in two successive steps. Firstly, the total amplitude at isosbestic point 255.4 nm of the ratio spectra of the mixture was measured representing the total actual concentration of both drugs in the mixture. Then, the first derivative of the ratio spectra was obtained to determine Hydrochlorothiazide concentration at 233 nm. While the concentration of Candesartan was determined subsequently by subtracting the Hydrochlorothiazide concentration calculated after derivatization from the total concentration of both drugs obtained at the ratio spectra before the derivatization step. Results: The SIDD was successfully applied for simultaneous determination of both drugs in their pure form or in their binary mixture either in synthetic prepared mixtures or in combined dosage form the adopted method was validated according to the ICH guidelines and the results were found to be within the acceptable limits. Conclusion: The adopted method highlighted the important role of normalized spectrum when used as a divisor in addition to the importance of isosbestic point to resolve severely overlapped spectra. All the measurements were carried using ethanol which is considered one of the greenest solvents making the method an environmentally friendly one. the adopted method was validated according to the ICH guidelines and the results were found to be within the acceptable limits.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND TAPENTADOL IN TABLETS BY RATIO SPECTRA DERIVATIVE SPECTROPHOTOMETRY

2021 ◽  
Vol 12 (9) ◽  
pp. 27-32
Author(s):  
Shah Esha Bhavin ◽  
Gajjar Anuradha
Keyword(s):  
Absorption Spectrum ◽  
Binary Mixture ◽  
Simultaneous Determination ◽  
Derivative Spectrophotometry ◽  
Pharmaceutical Tablets ◽  
First Derivative ◽  
Standard Spectrum ◽  
Ich Guidelines ◽  
Relative Standard

The application of the ratio spectra derivative spectrophotometry to the simultaneous determination of Paracetamol (PCM) and Tapentadol (TAP) in combined pharmaceutical tablets is presented. The spectrophotometric procedure is based on the use of the first derivative of the ratio spectra obtained by dividing the absorption spectrum of the binary mixtures by a standard spectrum of one of the compounds. The first derivative amplitudes were measured at 220 and 232 nm for the assay of TAP and PCM, respectively. Calibration graphs were established for 1-5 μg mL-1 for TAP and 6.5-32.5 μg mL-1 for PCM in binary mixture. The detection limits for TAP and PCM were found 0.098 and 0.595 μg mL-1, respectively, while the quantification limits were 0.298 μg mL-1 for TAP and 1.805 μg/ml for PCM. The relative standard deviations were found to be less than 2%, indicating reasonable repeatability of both methods. The proposed methods were hence validated as per ICH guidelines and successfully applied to the determination of these drugs in commercial tablets.

scholarly journals Simultaneous Determination of Caffeine, 8-Chlorotheophylline, and Chlorphenoxamine Hydrochloride in Ternary Mixtures by Ratio-Spectra Zero-Crossing First-Derivative Spectrophotometric and Chemometric Methods

2005 ◽  
Vol 88 (4) ◽  
pp. 1126-1134 ◽  
Author(s):  
Khadiga M Kelani
Keyword(s):  
Simultaneous Determination ◽  
Principal Component Regression ◽  
Detection Limits ◽  
Principal Component ◽  
Ternary Mixtures ◽  
Chemometric Methods ◽  
Zero Crossing ◽  
First Derivative ◽  
Preliminary Separation

Abstract A ratio-spectra zero-crossing first-derivative spectrophotometric method and 2 chemometric methods have been used for the simultaneous determination of ternary mixtures of caffeine (A), 8-chlorotheophylline (B), and chlorphenoxamine hydrochloride (C) in bulk powder and dosage forms. In the ratio-spectra zero-crossing first-derivative spectrophotometric technique (1DD), calibration curves were linear in the range of 4–20 μg/mL for A, B, and C (r = 0.9992, 0.9994, and 0.9976, respectively). The measurements were carried out at 212, 209.2, and 231.4 nm for A, B, and C, respectively. The detection limits for A, B, and C were calculated to be 0.24, 0.34, and 0.13 μg/mL, and the percentage recoveries were 99.1 ± 0.89, 100.1 ± 0.95, and 100.1 ± 1.0, respectively. Two chemometric methods, namely, the partial least-squares (PLS) model and the principal component regression (PCR) model, were also used for the simultaneous determination of the 3 drugs in the ternary mixture. A training set consisting of 15 mixtures containing different ratios of A, B, and C was used. The concentration used for the construction of the PLS and PCR models varied between 4 and 25 μg/mL for each drug. These models were used after their validation for the prediction of the concentrations of A, B, and C in mixtures. The detection limits for A, B, and C were calculated to be 0.13, 0.15, and 0.14 μg/mL, respectively, and the percent recoveries were found to be 99.8 ± 0.96, 99.9 ± 0.94, and 99.9 ± 1.18, respectively, for both methods. The 3 proposed procedures are rapid, simple, sensitive, and accurate. No preliminary separation steps or resolution equations are required; thus, they can be applied to the simultaneous determination of the 3 drugs in commercial tablets and suppositories or in quality-control laboratories.

APPLICATION OF RATIO DERIVATIVE SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS DETERMINATION OF ARTEMISININ AND CURCUMIN

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 43-47
Author(s):  
R Dhankecha ◽  
◽  
A Soni ◽  
M Gohel ◽  
V Thakkar ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Absorption Spectra ◽  
Spectrophotometric Method ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Direct Absorption ◽  
Acceptable Limit ◽  
First Derivative ◽  
Ich Guidelines

Ratio derivative spectrophotometric method has been developed for the simultaneous determination of artemisinin and curcumin. The overlapping spectra of both drugs were resolved by making use of the first-derivative of the ratios of their direct absorption spectra. The derivative ratio absorbances of artemisinin and curcumin were measured at λmax 293.17 and λmax 457.0 nm, respectively, for their quantification. Artemisinin and curcumin were determined in the concentration range of 2-10 μg/mL and 1-5 μg/mL, respectively. The method was validated as per the ICH guidelines and accuracy, precision were found to be within acceptable limit. The limits of detection and quantitation were found to be 0.003299 and 0.009997 μg/mL, respectively for artemisinin and 0.006743 and 0.020434 μg/mL, respectively for curcumin. The proposed ratio first derivative spectrophotometric method is novel, rapid, simple, sensitive, accurate, precise and successfully applicable for simultaneous estimation of artemisinin and curcumin in parentral dosage form.

scholarly journals A HPLC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF NIFEDIPINE AND ENALAPRIL IN HUMAN PLASMA

2018 ◽  
Vol 10 (4) ◽  
pp. 35 ◽  
Author(s):  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the simultaneous quantification of nifedipine and enalapril in human plasma.Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: The total chromatographic run time was 2.5 min and the elution of nifedipine, enalapril and IS (verapamil) occurred at ~1.83, 1.57 and 1.61 min, respectively. A linear response function was established at 1-100 ng/ml for nifedipine and 2-200 ng/ml for enalapril maleate in human plasma. The % mean recovery for enalapril in LQC, MQC and HQC was 114.0 %, 112.9 % and 113.2 %, for nifedipine in LQC, MQC and HQC was 104.1 %, 105.0 % and 108.7 % respectively. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 2.16 ng/ml for enalapril, 1.01 ng/ml for nifedipine. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 108.2 % for enalapril and 100.5 % for nifedipine, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 3.2 % and 7.4 % respectively, which are within 20.00% of the acceptance criteria.Conclusion: A rapid method was developed for simultaneous determination of nifedipine and enalapril in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine examination of nifedipine and enalapril in human plasma. 

scholarly journals Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation

2017 ◽  
Vol 2017 ◽  
pp. 1-8 ◽  
Author(s):  
Hanan A. Merey ◽  
Mahmmoud S. Abd-Elmonem ◽  
Hagar N. Nazlawy ◽  
Hala E. Zaazaa
Keyword(s):  
Simultaneous Determination ◽  
Pharmaceutical Dosage Form ◽  
Factors Affecting ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Flunixin Meglumine ◽  
Veterinary Pharmaceutical ◽  
Ich Guidelines ◽  
The Difference

Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY) and Flunixin Meglumine (FLU). The first method, dual wavelength (DW), depends on measuring the difference in absorbance (ΔA 273.4–327 nm) for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7–275.7 nm. The second method, first-derivative spectrophotometric method (1D), depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5–324.8 nm and ΔP 249.6–286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD), depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones.

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