scholarly journals Synthesis of Cyanuric Chloride based Chiral Reagent for RP-HPLC Enantioseparation of (RS)-Propranolol

2022 ◽  
Vol 34 (2) ◽  
pp. 376-382
Author(s):  
H.S. Al-Shehri ◽  
V. Alwera ◽  
K.C. Nilugal ◽  
S. Alwera
Keyword(s):  
Dft Calculations ◽  
Present Method ◽  
Chiral Recognition ◽  
Cyanuric Chloride ◽  
Chiral Reagent ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Ft Ir ◽  
Proline Derivatives ◽  
Derivatives Of

In this work, four cyanuric chloride based chiral reagents were prepared via nucleophile substitution of chlorine atom by L-proline derivatives and characterized by UV, FT-IR, HRMS, NMR and elemental analysis. Racemic propranolol was chosen for the chiral recognition study. The prepared chiral reagents were used in the synthesis of diastereomeric derivatives of (RS)-propranolol, under microwave heating conditions. RP-HPLC was used to separate the prepared diastereomeric derivatives. The effect of varying eluting phase concentrations and sample concentrations was optimized. The DFT calculations were performed using Gaussian 09 Rev A.02 to create the lowest energy optimised structures of diastereomeric derivatives. LOD (0.324 ng mL-1), LOQ (0.972 ng mL-1), calibration range (0.02-2.0 mg mL-1), correlation-coefficient (0.999), and recovery were the validation parameters for the present method (99.09 and 99.81 % for inter-day assay and 98.47 and 99.72 % for intra-day assay).

FT-IR, FT-Raman spectra and ab initio HF and DFT calculations of 4-N,N′-dimethylamino pyridine

2008 ◽  
Vol 71 (3) ◽  
pp. 898-906 ◽  
Author(s):  
N. Sundaraganesan ◽  
S. Kalaichelvan ◽  
C. Meganathan ◽  
B. Dominic Joshua ◽  
J. Cornard
Keyword(s):  
Dft Calculations ◽  
Ab Initio ◽  
Raman Spectra ◽  
Ft Ir ◽  
Hf And Dft Calculations ◽  
Ab Initio Hf ◽  
Ft Raman

scholarly journals New derivatives of a natural nordentatin

2020 ◽  
Vol 18 (1) ◽  
pp. 890-897 ◽  
Author(s):  
Tin Myo Thant ◽  
Nanik Siti Aminah ◽  
Alfinda Novi Kristanti ◽  
Rico Ramadhan ◽  
Hnin Thanda Aung ◽  
...  
Keyword(s):  
Cell Line ◽  
Parent Compound ◽  
T47d Cell ◽  
Positive Control ◽  
Inhibition Assay ◽  
Anticancer Activities ◽  
Methanol Fraction ◽  
T47d Cell Line ◽  
Ft Ir ◽  
Derivatives Of

AbstractNew derivatives were obtained from natural nordentatin (1) previously isolated from the methanol fraction of Clausena excavata by an acylation method. Herein, we report ten new pyranocoumarin derivatives 1a–1j. Their structures were elucidated based on UV-vis, FT-IR, NMR, and DART-MS data. The α-glucosidase inhibition and anticancer activities of nordentatin (1) and its derivatives were also evaluated. The α-glucosidase inhibition assay exhibited that the derivatives 1b, 1d, 1e, 1f, 1h, 1i, and 1j possess higher inhibitory activity for α-glucosidase with IC50 values of 1.54, 9.05, 4.87, 20.25, 12.34, 5.67, and 2.43 mM, whereas acarbose was used as the positive control, IC50 = 7.57 mM. All derivatives exhibited a weak cytotoxicity against a cervical cancer (HeLa) cell line with the IC50 between 0.25 and 1.25 mM. They also showed moderate to low growth inhibition of a breast cancer (T47D) cell line with IC50 values between 0.043 and 1.5 mM, but their activity was lower than that of the parent compound, nordentatin (1) (IC50 = 0.041 mM).

New Ferrocene-Integrated Multifunctional Guanidine Surfactants: Synthesis, Spectroscopic Elucidation, DNA Interaction Studies, and DFT Calculations

2021 ◽  
Author(s):  
Sameen Nawaz ◽  
Faiza Asghar ◽  
Jahangeer Patujo ◽  
Saira Fatima ◽  
Babar Murtaza ◽  
...  
Keyword(s):  
Dft Calculations ◽  
Atomic Absorption ◽  
Absorption Spectroscopy ◽  
13C Nmr ◽  
Atomic Absorption Spectroscopy ◽  
Analytical Methods ◽  
Dna Interaction ◽  
Interaction Studies ◽  
Ft Ir

Three new ferrocene-substituted aliphatic guanidines were successfully synthesized and well characterized by means of several analytical methods such as: FT-IR, 1H & 13C-NMR, Raman, atomic absorption spectroscopy (AAS), and elemental...

One new and six known triterpene xylosides from Cimicifuga racemosa: FT-IR, Raman and NMR studies and DFT calculations

2012 ◽  
Vol 93 ◽  
pp. 10-18 ◽  
Author(s):  
Marta K. Jamróz ◽  
Michał H. Jamróz ◽  
Jan Cz. Dobrowolski ◽  
Jan A. Gliński ◽  
Michał Gleńsk
Keyword(s):  
Dft Calculations ◽  
Cimicifuga Racemosa ◽  
Nmr Studies ◽  
Ft Ir

CP-MAS and FT-IR spectroscopic studies of new derivatives of gossypol in solid

2005 ◽  
Vol 751 (1-3) ◽  
pp. 151-155 ◽  
Author(s):  
Piotr Przybylski ◽  
Grzegorz Bejcar ◽  
Wojciech Schilf ◽  
Bogumil Brzezinski ◽  
Franz Bartl
Keyword(s):  
Spectroscopic Studies ◽  
Ft Ir ◽  
Ir Spectroscopic ◽  
Derivatives Of

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ENTECAVIR IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY RP-HPLC

2017 ◽  
pp. 107-111
Author(s):  
Swathi P. ◽  
S. Vidyadhara ◽  
R. L. C. Sasidhar ◽  
K. Kalyan Chakravarthi
Keyword(s):  
Flow Rate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Degradation Studies

Objective: The objective and purpose of the analysis have sensibly assessed by selecting of a rapid and sensitive RP-HPLC method for Entecavir in bulk and pharmaceutical dosage form by using the most commonly employed C-18column with UV detection.Methods: In estimation by RP-HPLC method Agilent 1120 compact LC system with variable programmable UV detector and Rheodyne injector with 20 µl fixed loop was used for the chromatographic separation. The mode of operation was isocratic with the components of a solution consisting of methanol: acetonitrile(70:30v/v) and triethanolamine (2-4drops)at the flow rate of 1.2 ml/min and run time was 10 min. Forced degradation studies were conducted to evaluate the stability and specificity of the method along with the validation parameters.Results: Validation parameters of HPLC were found at a detection wavelength of 255 nm. Linearity was observed with the concentration range (Beer’s law range) 20-100µg/ml with R2=0.9991. Robustness with detection wavelengths 253 and 257 nm with a flow rate of 1 ml/min and 1.4 ml/min showed good results. The retention time of the drug was 2.64 min and assay showed 98.1%.Conclusion: The proposed RP-HPLC method was validated as per the ICH Q2B Guidelines, and was found to be applicable for routine quantitative analysis of Entecavir by RP-HPLC using UV detector in pharmaceutical dosage forms. The results of linearity, precision, accuracy and specificity, were proved, that does not exceed certain specified limits. The method provides selective quantification with no interference from other formulation excipients. The proposed method was highly sensitive, reproducible, reliable, robust and specific. Therefore, this method is a simple, rapid analysis may actually be more desirable than a more complicated and time-consuming process. The degradation studies at various stress conditions like thermal and hydrolytic, drug gets degraded at a temperature of 80 °c and refluxing with water at 70 °c for 24hours. 

scholarly journals SIMULTANEOUS DETERMINATION OF DIPHENHYDRAMINE, EPHEDRINE, NOSCAPINE, AND GLYCEROL GLYCOLATE USING STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY: APPLICATION TO NOSCOF TABLETS

2019 ◽  
pp. 505-511
Author(s):  
PULAGURTHA BHASKARARAO ◽  
GOWRI SANKAR DANNANA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Uv Light ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters

Objective: Noscof tablet is a fixed dosage combination formulation having diphenhydramine (DH), ephedrine (ED), noscapine (NP), and glycerol glycolate (GG). A sensitive, selective, accurate, precise, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method with photodiode array detection has been developed and validated for simultaneous analysis of DH, ED, NP, and GG in bulk drug and Noscof tablets. Methods: Reversed-phase chromatographic separation and analysis of DH, ED, NP, and GG were done on an Altima C18 column with 0.01 M KH2PO4 buffer (pH 3.5) and acetonitrile (50:50%, v/v) as mobile phase at 0.8 ml/min flow rate in isocratic mode. Detection was performed at 260 nm. The method was validated in harmony with International Conference on Harmonization (ICH) guidelines. The tablet sample solution was subjected to diverse stress conditions using ICH strategy such as hydrolytic degradation (neutral - with distilled water, alkaline - with 2 N NaOH, and acidic - with 2 N HCl), oxidation (with 10% H2O2), photodegradation (exposing to UV light), and dry heat degradation (exposing to 105°C). Results: Using the above stated chromatographic conditions, sharp peaks were obtained for ED, NP, DH, and GG with retention time of 3.272 min, 4.098 min, 5.467 min, and 6.783 min, respectively. Good regression coefficient values were obtained in the range of 2–12 μg/ml for ED, 3.75–22.5 μg/ml for NP, 3.125–18.75 μg/ml for DH, and 25–150 μg/ml for GG. The quantification limits were 0.181 μg/ml, 0.187 μg/ml, 0.246 μg/ml, and 1.114 μg/ml for ED, NP, DH, and GG, respectively. The values of validation parameters are within the acceptance limits given by ICH. The ED, NP, DH, and GG showed more percent of degradation in acid condition and less percent of degradation in the neutral condition. The peaks of degradants did not interfere with the peaks of analytes. ED, NP, DH, and GG were assessed with a good percentage of the assay (near to 100%) and low percent relative standard deviation (<2%) in Noscof tablets using the proposed method. Conclusion: The stability indicating RP-HPLC method developed was suitable for quantifying ED, NP, DH, and GG simultaneously in bulk as well as in tablet formulation.

scholarly journals Synthesis, characterization and Cytotoxicity Evaluation of New Heterocyclic Compounds with Oxazole Ring Containing 4-(Phenylsulfonyl)phenyl Moiety

2019 ◽  
Vol 70 (11) ◽  
pp. 3793-3801
Keyword(s):  
Therapeutic Potential ◽  
Hplc Method ◽  
Oxazole Ring ◽  
Acyl Chlorides ◽  
Rp Hplc ◽  
Toxicological Profile ◽  
Ft Ir ◽  
Cytotoxicity Assessment ◽  
New Compounds

The paper presents the synthesis, characterization and cytotoxicity assessment of five organic compounds containing 4-(phenylsulfonyl)phenyl fragment in the molecule, namely of three acyclic precursors derived from phenylalanine (from N-acyl-a-amino acids, N-acyl-a-amino acyl chlorides and N-acyl-a-amino ketones class) and of the cyclization products: a 1,3-oxazol-5(4H)-one and, respectively, a 1,3-oxazole substituted in position 5 with the p-tolyl group. The synthesized compounds were characterized by spectral methods (UV-Vis, FT-IR, 1H-NMR, 13C-NMR, and MS) and elemental analysis, which confirmed their structures. For the determination of the purity of the new compounds, the RP-HPLC method was used. In view of the therapeutic potential of the newly synthesized compounds, we evaluated their toxicological profile using the Daphnia magna bioassay. Keywords: N-acyl-a-amino acid, 1,3-oxazol-5(4H)-one, N-acyl-a-amino ketone, 1,3-oxazole, cytotoxic effect

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