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1.
Spectrochim Acta A Mol Biomol Spectrosc ; 318: 124467, 2024 Oct 05.
Artigo em Inglês | MEDLINE | ID: mdl-38796892

RESUMO

The study aimed to determine the potential of the infrared (IR) spectrophotometric technique for measuring the content of sulphanilamide with the sulfonamide group. The study aimed to obtain the IR spectra of sulfanilamide and use the -SO2 band at 1114.37 for the quantitative assay, determining its area under the curve (AUC). The study gives an alternative approach to existing analytical techniques that require vast amounts of organic solvents, which are costly and can be toxic, thus impacting the environment and increasing the analysis cost. The study evaluated the method's whiteness and greenness by utilizing the Complex green analytical procedure index, analytical GREEness calculator and Red Green Blue algorithm tool. The linierity was found to be 5 to 30 µg/ml. The present study has developed an infrared (IR) spectroscopic method that employs a straightforward sample preparation technique in methanol. The IR spectroscopic method's linearity range was determined to be 5-30 µg/ml. The p-value was 0.001 at 95 % confidence level assuring better recovery. This method is evaluated according to the Q2R1 ICH guideline. It is applicable to routine quality control analysis without pre-extraction using green IR spectroscopy. In conclusion, the study demonstrated that IR spectrophotometric techniques can quantify sulfanilamide while reducing the use of organic solvents, contributing to the green-and-white analytical chemistry approach. The developed methods are reliable, accurate, and cost-effective and have the potential to be implemented in routine analysis of sulfanilamide.


Assuntos
Espectrofotometria Infravermelho , Sulfanilamida , Sulfanilamida/análise , Sulfanilamida/química , Espectrofotometria Infravermelho/métodos , Sulfanilamidas/análise , Sulfanilamidas/química , Algoritmos , Reprodutibilidade dos Testes
2.
J Chromatogr Sci ; 2024 May 22.
Artigo em Inglês | MEDLINE | ID: mdl-38776060

RESUMO

In this study, a sustainable and eco-friendly method is developed to quantify azelnidipine and chlorthalidone in rabbit plasma by gradient liquid chromatography based on green chemistry principle and analytical quality by design. The separation was achieved on a Shim pack C18 (25 cm × 5 cm × 4.6 µm) column with L1 packing. The mobile phase compromised of ethanol and 50-Mm ammonium acetate buffer (pH.6) at flow rate of 0.6 mL/min with 25-min runtime. The resolution and asymmetric factor were identified as critical analytical attributes (CAAs). The screening studies employing Control Noise Experimentation revealed that mobile phase pH, flow rate and ethanol concentration at 6 and 15 min significantly affected the CAAs method. The critical method parameters were optimized using Central Composition design. Chromatogram showed peak of the drugs at retention time of 9.03 min for chlorthalidone and 16.83 min for azelnidipine. The greenness score of the analytical method was found to be 1876.43 using analytical method greenness score calculator. The validation of the developed method was done which showed linearity at the range of 16-520 ng/mL, with R2 of 0.9992 and 0.9996 for azelnidipine and chlorthalidone, respectively, furthermore accuracy, precision, recovery and stability studies are carried out.

3.
J Chromatogr Sci ; 59(7): 627-633, 2021 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-33912904

RESUMO

A simple, precise, rapid and accurate UFLC method has been developed with due validation for the simultaneous estimation of Amlodipine besylate and Celecoxib in rat plasma. The separation has been taken place by C18 Eclipse plus column at 1ml/min flow rate. The mobile phase comprises of 20 mM sodium acetate buffer of pH 4.5 adjusted with glacial acetic acid and methanol (30:70% v/v). The effluents were monitored at 228 nm with a total run time of 15min. The retention time of Amlodipine besylate and celecoxib were found to be 7.69 min and 10.69 min respectively. The extraction of drugs have been achieved by protein precipitation technique with methanol as a solvent. The detection concentration was linear over 60-420 ng/ml for Amlodipine besylate and 600-4200 ng/ml for Celecoxib. Regression equation of Amlodipine besylate and Celecoxib were found to be y = 30.996x + 520.29 & y = 39.722x + 23706 with regression coefficient 0.9944 & 0.9941 respectively using unweighted and weighted linear regression with a weighting factor of 1/x0, 1/x, 1/✓x and 1/x2. The percentage recoveries were found to be 88.52±1.276 to 93.06±2.872 for Amlodipine & 89.40±0.728 to 94.05±0.221 for Celecoxib. This liquid chromatography method was extensively validated for linearity, accuracy precision, and stability studies.


Assuntos
Anlodipino/sangue , Celecoxib/sangue , Cromatografia Líquida de Alta Pressão/métodos , Animais , Feminino , Modelos Lineares , Masculino , Ratos , Ratos Wistar , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
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