Derivative Spectroscopic Method Research Articles

Estimation and Validation of Vidagliptin by First Order Derivative Spectroscopy Method.

A method has been successfully developed for the simultaneous estimation of Vildagliptin in both its bulk drug and tablet dosage form. The drug exhibits absorbance maxima at 228 nm in a 0.1N NaOH solution, and conforms to Beer’s law within a concentration range of 10-50 µg/ml. The mean recovery rate for both the bulk drug and tablet form was determined to be 100%, indicating the method's efficacy in accurately retrieving the expected quantities of the drugs. Furthermore, the method demonstrated linearity close to 1, suggesting a strong correlation between concentration and absorbance, which is crucial for precise quantification. Assessment of precision through various parameters including intraday, interday, and intermediate precision, as well as robustness, yielded consistent results. The percentage recovery fell within the acceptable range of 82-138% for both drugs, further affirming the method's accuracy and reproducibility. Importantly, all validation parameters were found to be in compliance with the guidelines set forth by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH), ensuring the method's adherence to industry standards. In conclusion, these findings collectively underscore the accuracy, precision, and simplicity of the developed method for the simultaneous estimation of Vildagliptin bulk drug and its tablet dosage form.

Estimation and Validation of Sitagilptin by First Order Derivative Spectroscopy Method

A method has been successfully developed for the simultaneous estimation of Sitagilptin in both its bulk drug and tablet dosage form. The drug exhibits absorbance maxima at 228 nm in a 0.1N NaOH solution, and conforms to Beer’s law within a concentration range of 10-50 µg/ml. The mean recovery rate for both the bulk drug and tablet form was determined to be 100%, indicating the method's efficacy in accurately retrieving the expected quantities of the drugs. Furthermore, the method demonstrated linearity close to 1, suggesting a strong correlation between concentration and absorbance, which is crucial for precise quantification. Assessment of precision through various parameters including intraday, interday, and intermediate precision, as well as robustness, yielded consistent results. The percentage recovery fell within the acceptable range of 82-138% for both drugs, further affirming the method's accuracy and reproducibility. Importantly, all validation parameters were found to be in compliance with the guidelines set forth by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH), ensuring the method's adherence to industry standards. In conclusion, these findings collectively underscore the accuracy, precision, and simplicity of the developed method for the simultaneous estimation of Sitagilptin bulk drug and its tablet dosage form

A Novel Uv Spectrophotometric Method Development and Validation of Dalfampridine in Bulk and Pharmaceutical Dosage Form

Simple, precise and accurate zero order derivative spectroscopic method has been developed and validated for the estimation of dalfampridine in bulk and pharmaceutical dosage form. The drug shows maximum absorption (λ max) at 262nm in 0.1M HCL and obeys Beer’s law in the concentration range of 0.5-3.0µg/ml. The linearity study was carried out and regression coefficient was found to be 0.9976 and it has showed good linearity, precision during this concentration range. The % recovery was found to be 98.66% -101.56%. The LOD and LOQ were found to be 0.0360 and 0.109µg/ml. The % relative standard deviation were found to be less than 2. According to ICH guidelines the technique has been validated for linearity, precision, accuracy, ruggedness, LOD and LOQ. The developed and validated method can be successfully applied for routine quantification of Dalfampridine in bulk and pharmaceutical dosage form.

Simultaneous Determination of Pyridoxine HCl, Isoniazid, Trimethoprim and Sulfamethoxazole by Double Divisor Ratio Spectra Derivative Spectroscopic Method

Tuberculosis could be regarded as a serious and enduring menace to global health. A significant hurdle in tuberculosis treatment lies in drug resistance, including the emergence of multiple drug resistance. A regulatory agency has recently endorsed the fixed-dose combination of pyridoxine HCl, isoniazid, trimethoprim, and sulfamethoxazole as a robust therapy for cases of tuberculosis resistant to multiple drugs. Therefore, a successful attempt was made to develop and validate a novel spectroscopic method, i.e., double deviation ratio spectra derivative spectroscopic method, for the simultaneous determination of pyridoxine HCl, Isoniazid, trimethoprim, and sulfamethoxazole in their pure form. The optimized divisor concentration in the developed method was found to be a mixture of 6 μg/mL of sulfamethoxazole and 16 μg/mL of pyridoxine HCl for the determination of isoniazid and trimethoprim in the same quaternary mixture. Similarly, the optimized divisor concentration for the determination of sulfamethoxazole and pyridoxine HCl was found to be a mixture of isoniazid and trimethoprim with concentrations of 10 and 12 μg/mL, respectively. With the developed method, the linearity for pyridoxine HCl, isoniazid, trimethoprim, and sulfamethoxazole was found to be in the range of 8 to 40 μg/mL, 10 to 30 μg/mL, 12 to 36 μg/mL, and 4 to 12 μg/mL, respectively. The results of the accuracy study, in terms of percentage recovery, were found to be 99.92 ± 0.978, 100.04 ± 1.731, 99.87 ± 1.811, and 98.83 ± 0.922 for the simultaneous determination of pyridoxine HCl, isoniazid, trimethoprim, and sulfamethoxazole, respectively, using the developed method. The developed method has been successfully validated as per the ICH guidelines.

Simultaneous UV-Visible Spectrophotometric Determination of Nelfinavir and Quercetin in Patented Pharmaceutical Formulation and Bulk by First-Order Derivative Spectroscopic Method

Simultaneous UV-Visible Spectrophotometric Determination of Nelfinavir and Quercetin in Patented Pharmaceutical Formulation and Bulk by First-Order Derivative Spectroscopic Method

Graphitic carbon nitride-adorned PDMS self-cleaning floating photocatalyst for simultaneous removal of Rhodamine B, Crystal Violet and Malachite Green from a ternary dye mixture.

Graphitic carbon nitride-adorned polydimethylsiloxane (PDMS) floating catalyst was prepared by a simple procedure. The prepared catalyst was utilized for the simultaneous mitigation of recalcitrant organic pollutants such as Rhodamine B, Crystal Violet and Malachite Green from their ternary mixture for the first time. Derivative spectroscopic method was used to calculate the degradation efficiencies of individual dyes in the mixture. The prepared catalyst showed a consistent degradation performance up to 4 cycles inducing a degradation of 94.02%, 92.1% and 97.13% of Rhodamine B, Crystal Violet and Malachite Green, respectively, in a dye(s) solution with a catalytic loading of 0.5g L-1. A kinetic analysis of the dye(s) degradation under visible light was carried out during the course of this work up to 120min. A detailed characterization of the surface of this novel catalyst was carried out in this study by SEM, EDX, XRD, DRS, DTG, FTIR, Raman spectroscopy and UV-Vis spectroscopy and provided the experimental proof for the catalyst presenting high hydrophobicity, self-cleaning ability, good recyclability and high chemical stability.

Determining relative values of pH, CECe, and OC in agricultural soils using functional enhanced derivative spectroscopy (FEDS0) method in the mid-infrared region

Soils are a vital and non-renewable natural resource that provide the nutrients and adequate conditions for plants growth, as well to support several economic activities. Optical spectroscopy has emerged as a reliable technique for determining multiple physicochemical properties of organic and inorganic species in agricultural industries, that employs mathematical and statistical tools to develop new methodologies of spectral analysis easily implementable in remote and in-field applications. This is the case of the Functionally-enhanced derivative spectroscopy (FEDS and FEDS0), which uses operational transformations to extract hidden information from overlapping optical signals generated by the diverse components of solid and liquid matrices. In this study, an algorithm based on FEDS has been applied for optical analysis of agricultural soils in the spectral range from 1200 to 675 cm−1, to estimate chemical properties related to nutritional and fertility state of 65 soil samples used for planting of cotton, yuca (Manihot Esculenta), and banana in Bolivar and Cordoba departments in Colombia. The results demonstrate that it is possible to establish a correlation between the Pearson’s coefficient obtained from two FEDS0 spectra associated to ATR-FTIR signals (rF > - 0.85), and their relative values of effective cation exchange capacity, pH and organic carbon content, with a ratio of performance to deviation higher to 2.0 in all cases (RPD > 2.0). This is possible due to high dependence of optical signal with CECe values, which are in turn conditioned by pH level and OC content in the soil samples considered.

A New Zero Cross Technique for Simultaneous Estimation of Rosuvastatin Calcium and Fenofibrate in Tablets by UV Derivative Spectroscopic Method

A New Zero Cross Technique for Simultaneous Estimation of Rosuvastatin Calcium and Fenofibrate in Tablets by UV Derivative Spectroscopic Method

Derivative Spectroscopic Method and RP-HPLC Method Development and Validation of Levofloxacin hemihydrate

The present work describes the development of a simple, precise and accurate derivative spectroscopic and RP-HPLC method for the estimation of levofloxacin hemihydrate in the tablet dosage form. Levofloxacin hemihydrate showed absorption maxima at 287.36, 287.2 and 296.2nm in zero, first and second-order spectroscopic methods. The RP-HPLC method was optimized by using Orthophosphoric acid: acetonitrile: methanol (50: 20: 30) as solvent at 287nm. The methods showed linearity in the concentration range 1-5 and 2-10 µg/ ml and the correlation coefficient was 0.999 respectively. The method has been validated according to the ICH guidelines. The percentage relative standard deviation was found to be less than 2% in respect of both methods.

Determination of Cefuroxime Axetil in Tablet by HPLC, UV and First-Order Derivative Spectroscopy Methods & Plasma by UV Spectroscopy Method

It was aimed to develop and validate the UV spectroscopic, the first-order derivative spectroscopy, and the HPLC method for determination of cefuroxime axetil in bulk and tablets and also in spiked human plasma samples by UV spectroscopy method. In the spectroscopic analyses, the maximum absorbance of cefuroxime axetil in acetonitrile was obtained at 277 nm wavelength in the spectra. In first-order derivative spectroscopy method, two peaks were observed in spectra, a maximum at 258 nm and a minimum at 298 nm. 298 nm wavelength was used in the study. In HPLC-UV study, parameters were chosen as follows: C18 column, 0.1% acetic acid-acetonitrile (30:70; v/v) for mobile phase, 1.0 mL/min of flow rate, 280 nm of wavelength, 10 μL of injection volume and etodolac (2.5 μg/mL) as internal standard. Accuracy, precision, recovery, linearity and sensitivity parameters were determined for each of the three methods. Developed and validated methods were successfully applied on 4 tablets which are named as Cefaks, Cefurol, Aksef ve Enfexia. As a result, it is claimed that proposed method is sensitive, precise, accurate, and successfully used in quality control studies in the drug industry.

INVESTIGATION OF PHOTOLUMINESCENCE OF ZnSxSe1-x AND ZnSxSe1-x:Mn NANOCRYSTALS OBTAINED BY COMBUSTION SYNTHESIS FOR OPTOELECTRIC DEVICES

The photoluminescence spectra of ZnSxSe1-x and ZnSxSe1-x : Mn nanocrystals obtained by combustion synthesis for all compositions with the parameter step x = 0.2 were registered. The movement of the maximum of the integral photoluminescence spectrum in ZnSxSe1-x and ZnSxSe1-x : Mn nanocrystals towards higher energies, depending on the parameter x, was noted. It was noticed that in the range of values x = 0.2÷0.4 there is an abrupt change in the half-width of the integral photoluminescence spectrum in ZnSxSe1-x and ZnSxSe1-x : Mn nanocrystals and the signal intensity; this may be due to the crystal lattice transformation. The parameters of the individual photoluminescence spectra of ZnSxSe1-x : Mn nanocrystals were determined by one experimental measurement based on the Tikhonov method and the derivative spectroscopy method. The nature of the individual photoluminescence bands is discussed. The difference between the integral (sum of individual bands) and experimental spectrum arises from the presence of an additional individual band of low intensity in the experimental spectrum. This individual band is located in the region of E = 2.48 eV and is associated with the electronic transitions in Mn2+ ions in the ZnS lattice.

Development and Validation of Novel Analytical Method for Estimation of Diltiazem HCL

A novel, simple, accurate and precise Zero order derivative spectroscopic method was developed and validated for the estimation of Diltiazem HCl in bulk and Pharmaceutical dosage forms and has an absorption maximum at 193 nm in 0.05N Sulphuric acid. The Linearity was found to be in the concentration range of 3-18 μg/ml and the correlation coefficient was found to be 0.998 and it has showed good linearity, reproducibility, precision in this concentration range. The regression equation was found to be Y = 0.0971x + 0.0268 .The % recovery values were found to be within 99.3 -102.06 % showed that the method was accurate. The LOD and LOQ were found to be 0.222 and 0.675μg/ml, respectively. The % RSD values were less than 2. The method has been validated according to ICH guidelines for linearity, accuracy, precision, ruggedness, Limit of detection and limit of quantitation. Proposed method was successfully applied for the quantitative estimation of Diltiazem HCl in bulk and pharmaceutical dosage form.

Simultaneous Estimation of Abacavir Sulfate and Lamivudine in their Combined Dosage Form by First Derivative Zero-Crossing and Ratio First Derivative Spectroscopic Methods

Simultaneous Estimation of Abacavir Sulfate and Lamivudine in their Combined Dosage Form by First Derivative Zero-Crossing and Ratio First Derivative Spectroscopic Methods

A VALIDATED METHOD DEVELOPMENT FOR ESTIMATION OF BENDAMUSTINE HCL IN BULK AND SOLID DOSAGE FORM BY 1ST ORDER DERIVATIVE SPECTROSCOPY

This study aimed to expand the trouble-free, quick, cost-effective and sensitive 1st Order derivative spectroscopy method for bendamustine hydrochloride. The aliquot was scanned from 200-400 nm using blank methanol as a solvent and the absorption was recorded. The stored spectrum was modified into the first derivative spectrum by using UV probe software and the detection wavelength was selected as 269 nm in methanol. The linearity was considered more at the concentration range bearing 10-80 µg mL-1 with the regression equation established to be y = 0.001x+0.005 (R2 =0.998).The % RSD for intraday precision study was found to be 1.6043% and inter-day precision was found to be 1.3274%. System and method precision were determined to be less than 2%. LOD and LOQ were found to be 0.6435 µg and 1.9501 µg, respectively. The assay of the marketed formulations was found to be 99.78%. All of the validation parameters were found to be below 2% RSD. Hence, the method can be used for the estimation of bendamustine hydrochloride in bulk dosage forms and the method was validated as per ICH guidelines Q2(R1 ).

SIMULTANEOUS DETERMINATION OF VALSARTAN AND HYDROCHLOROTHIAZIDE BY FIRST-ORDER DERIVATIVE- ZERO CROSSING UV-VISIBLE SPECTROPHOTOMETRIC METHOD

Background: Antihypertensive drugs are widely used to treat high blood pressure in patients. The aim of this study is to prepare various mixtures of valsartan and hydrochlorothiazide, to create a matrix effect in the drug, and to determine the determination of these active substances in drug samples after optimum conditions by first-order derivative spectroscopy method.
 Method: In the first-degree derivative spectrophotometry method applied, valsartan and hydrochlorothiazide were dissolved in methanol and 100 mgL-1 solutions were prepared, and then the mixtures of these solutions were determined in spectrophotometry. After mixing, tablet (drug) sample was prepared and absorbance values were recorded and the first derivative spectrophotometric method was applied to the values obtained.
 Results: As a result of the spectrophotometric determination of various mixtures of valsartan and hydrochlorothiazide used in the study, it was determined that the first-order derivative spectrophotometric method applied gave very consistent results.
 Conclusion: The first-order derivative spectrophotometry method used in the study can be easily applied in routine analyzes in drug research laboratories.
 
 Peer Review History: 
 Received: 15 July 2022; Revised: 10 August; Accepted: 7 September, Available online: 15 September 2022
 Academic Editor: Dr. A.A. Mgbahurike, University of Port Harcourt, Nigeria, amaka_mgbahurike@yahoo.com
 UJPR follows the most transparent and toughest ‘Advanced OPEN peer review’ system. The identity of the authors and, reviewers will be known to each other. This transparent process will help to eradicate any possible malicious/purposeful interference by any person (publishing staff, reviewer, editor, author, etc) during peer review. As a result of this unique system, all reviewers will get their due recognition and respect, once their names are published in the papers. We expect that, by publishing peer review reports with published papers, will be helpful to many authors for drafting their article according to the specifications. Auhors will remove any error of their article and they will improve their article(s) according to the previous reports displayed with published article(s). The main purpose of it is ‘to improve the quality of a candidate manuscript’. Our reviewers check the ‘strength and weakness of a manuscript honestly’. There will increase in the perfection, and transparency. 
 Received file: Reviewer's Comments:
 Average Peer review marks at initial stage: 5.5/10
 Average Peer review marks at publication stage: 7.0/10
 Reviewers:
 Dr. U. S. Mahadeva Rao, Universiti Sultan Zainal Abidin, Terengganu Malaysia, raousm@gmail.com
 Prof. Cyprian Ogbonna ONYEJI, Obafemi Awolowo University, Ile-Ife, Nigeria, conyeji@oauife.edu.ng
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 UV SPECTROSCOPY DETERMINATION OF CILAZAPRIL AND HYDROCHLOROTHIAZIDE ACTIVE AGENTS USED IN THE TREATMENT OF HYPERTENSION

Development and Validation of UV and RP-HPLC Methods for Simultaneous Estimation of Mirabegron and Solifenacin Succinate in Their Pharmaceutical Dosage Form

Recently, a new formulation containing Mirabegron (MB) and Solifenacin succinate (SFS) has been approved for the management of over active bladder. However, only one analytical method has been reported for the simultaneous determination of both the analytes. Therefore, the current study was design to develop simple UV derivative spectroscopic and rapid RP-HPLC methods for simultaneous determination of MB and SFS. The chromatographic separation of MB and SFS was performed using Phenomenex Kinetex C18 (150mm × 4.5 mm × 5 µm) analytical column. A mixture of Water: Acetonitrile (20:80%v/v) was consider as mobile phase, at a flow rate of 1ml/min and at detector wavelength 225nm. A linear response was observe over the concentration range 2.5-12.5 µg/ml and 0.5-2.5 µg/ml respectively. The first order derivative method was develop by derivatisation of the zero absorption spectra for the first absorption spectra. The Zero crossing point of MB and SFS at 221 nm and 266 nm was obtain respectively. Beer’s law is obey in the concentration range of 7.5-20 µg/ml and 1.5-4 µg/ml for MB and SFS with correlation coefficient (R2) of 0.9984 and 0.9993 respectively. Both the methods were validated in accordance to guidelines for linearity, precision, repeatability, limit of detection (LOD), Limit of Quantification (LOQ), accuracy and robustness. Further, both the methods were validated and compared statistically using Student’s-t-test and employed for the concurrent estimation of MB and SFS in formulations. The proposed methods were simple, accurate, precise, and rapid. Therefore, they can be use for regular quality control of MB and SFS formulations and dissolution studies as well.

Sensitivity Enhanced Ecofriendly UV Spectrophotometric Methods for Quality Control of Telmisartan and Benidipine Formulations: Comparison of Whiteness and Greenness with HPLC Methods.

The development of an environmentally friendly analytical technique for simultaneous measurement of medicines with large concentration differences is difficult yet critical for environmental protection. Hence, in this work, new manipulated UV-spectroscopic methods with high scaling factors were established for concurrent quantification of telmisartan (TEL) and benidipine (BEN) in fixed-dose combinations. Two different methods were developed and established by calculation of peak height at zero crossing point of second derivative and the ratio of first derivative spectra with a scaling factor of 200 and 100, respectively. The absorption difference between the peaks and troughs of the ratio spectra, as well as continuous subtraction from ratio spectra, were established as additional methods. In addition, new procedures were validated using ICH recommendations. The proposed methods’ linearity curves were constructed in the range of 0.5–10 µg mL−1 and 1–30 µg mL−1 for BEN and TEL, respectively, under optimized conditions. Furthermore, both the detection (0.088–0.139 µg mL−1 for BEN and 0.256–0.288 µg mL−1 for TEL) and quantification limits (0.293–0.465 µg mL−1 for BEN and 0.801–0.962 µg mL−1 for TEL) were adequate for quantifying both analytes in the formulation ratios. The accuracy and precision were confirmed by the good recovery percent (98.37%–100.6%), with low percent relative error (0.67%–1.70%) and less than 2 percent relative standard deviation, respectively. The specificity of the methods was proven by accurate and precise outcomes from the standard addition method and analysis of laboratory mixed solutions with large differences in concentrations of both analytes. Finally, the BEN and TEL content of the formulations was determined simultaneously without prior separation using these first ever reported spectroscopic methods. Furthermore, developed UV derivative spectroscopic methods demonstrated high greenness and whiteness when compared to the reported HPLC methods. These findings show that the projected methods were effective, practical, and environmentally acceptable for quality control of BEN and TEL in multicomponent formulations.

Quantitative estimation of sitagliptin and dapagliflozin propanediol monohydrate in synthetic mixture using 1 order derivative spectroscopy simultaneous spectrophotometric analysis

Current research paper describes highly specific and reproducible 1 order derivative spectroscopic method for quantitative analysis of Sitagliptin which is a DPP4 inhibitors and Dapagliflozin which is SGLT2 inhibitors from its synthetic mixture. Both drugs are from Anti Diabetics class. Present analytical method was developed on Shimadzu double beam spectrophotometer equipped with UV probe 2.42 as software using methyl alcohol as solvent. Quantification of Sitagliptin was carried out at zero cross over point of Dapagliflozin that is 275 nm and for Dapagliflozin, it was achieved at 232 nm which is zero cross over point of Sitagliptin. Method shows linear response in the range of 25-125 µg/mL of Sitagliptin and 2.5-12.5 µg/mL of Dapagliflozin. Method was found to be accurate with recovery between 99.3 – 100.1 % for Sitagliptin and 98.2 – 100.7 % for Dapagliflozin. The developed method was validated as per ICH Q2 R1 guidelines and was successfully applied for quantitative analysis of synthetic mixture of Sitagliptin and Dapagliflozin.

Development and validation of derivative UV spectroscopic method for simultaneous estimation of nicotinamide and tretinoin in their binary mixtures and pharmaceutical preparations

An accurate, precise, sensitive, and simple spectroscopic method was developed and validated for simultaneous quantification analysis of tretinoin (TRT) and nicotinamide (NCT) with a ratio of 1:40 (TRT: NCT) in a synthetic mixture from dermal pharmaceutical preparations (solution and cream). Wavelengths were chosen in the first and second-order derivatives which are valid for the determination of NCT with the existence of TRT and excipients of the tested pharmaceutical preparations. Wavelength 253 nm was picked for the first-order derivative. Wavelengths 245 and 269 nm were picked for the second derivative. All previous wavelengths were zero-crossing points for TRT and its pharmaceutical preparations. Zero-order spectroscopy was used to determine TRT at the wavelength 348 nm, where no interference with NCT or any substance in the previous pharmaceutical preparation. The linearity range was studied and found to be 20–120 μg/mL and 0.5–5.0 μg/mL for NCT and TRT respectively. The correlation coefficient was 0.9995–0.9999 for NCT and 0.9998–0.9999 for TRT. The limit of detection (LOD) and the limit of quantification (LOQ) of NCT were 1.510 μg/mL and 4.590 μg/mL respectively at the wavelength 269 nm of the second-order derivative.

COMBINATION EFFECT OF LULICONAZOLE AND CLOBETASOL FOR TREATMENT OF SKIN AILMENTS

Objective: The new combination for Luliconazole and Clobetasol Propionate was approved for the treatment of a variety of skin disease. The main objective of this research is development and validation of novel, simple, fast and responsive derivative spectroscopic process for simultaneous estimation of newly approved combination Luliconazole (LLZ) and Clobetasol Propionate (CLP).
 Methods: Here in this first derivative spectroscopic method, the absorbance of LLZ and CLP was taken at 312 nm (ZCP of CLP) and 249 nm (ZCP of LLZ), respectively. Establishment of linearity was in a concentration varies from 10-50 µg/ml for Luliconazole and 5-25µg/ml for Clobetasole Propionate.
 Results: From the method developed above the R2 value observed for LLZ and CLP is 0.9961. Statistical validation of accuracy and reproducibility was done for planned procedure with the help of recovery studies. The mean % recovery of Luliconazole and Clobetasol Propionate was found to be 99.45 % and 99.43%, respectively. For LLZ the Limit of detection is 0.9988 µg/ml and limit of quantification is 0.0009µg/ml and for CLP the Limit of detection is0.0164µg/ml and limit of quantification 0.0027µg/ml.
 Conclusion: From research work the method development was done and shows fast, precise, exact and easy accessible laboratory procedure for routine evaluation of combination drugs.