scholarly journals Transition Metal Complexes of Naproxen: Synthesis, Characterization, Forced Degradation Studies, and Analytical Method Verification

2016 ◽  
Vol 2016 ◽  
pp. 1-10 ◽  
Author(s):  
Md. Sharif Hasan ◽  
Ruhul Kayesh ◽  
Farida Begum ◽  
S. M. Abdur Rahman

The aim of our current research was to synthesize some transition metal complexes of Naproxen, determine their physical properties, and examine their relative stability under various conditions. Characterizations of these complexes were done by 1H-NMR, Differential Scanning Calorimetry (DSC), FT-IR, HPLC, and scanning electron microscope (SEM). Complexes were subjected to acidic, basic, and aqueous hydrolysis as well as oxidation, reduction, and thermal degradation. Also the reversed phase high-performance liquid chromatography (RP-HPLC) method of Naproxen outlined in USP was verified for the Naproxen-metal complexes, with respect to accuracy, precision, solution stability, robustness, and system suitability. The melting points of the complexes were higher than that of the parent drug molecule suggesting their thermal stability. In forced degradation study, complexes were found more stable than the Naproxen itself in all conditions: acidic, basic, oxidation, and reduction media. All the HPLC verification parameters were found within the acceptable value. Therefore, it can be concluded from the study that the metal complexes of Naproxen can be more stable drug entity and offer better efficacy and longer shelf life than the parent Naproxen.

2020 ◽  
Vol 16 (7) ◽  
pp. 867-871
Author(s):  
Harun Ergen ◽  
Muge Guleli ◽  
Cigdem Sener ◽  
Cem Caliskan ◽  
Sercan Semiz ◽  
...  

Introduction: Polyvinyl alcohol (PVA), a polymer, is in demand due to its usage in different applications such as pharmaceutical, biomedical and textile, paper, food industries. Methods: A new sensitive reversed phased high-pressure liquid chromatography (RP-HPLC) method with refractive index detector (RID) was developed for determination of PVA in an ophthalmic solution containing dexpanthenol and PVA as active substances and it was validated according to The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guideline. Results: Chromatographic separation was achieved on a Chiral-AGP (150 mm × 4.0 mm, 5 μm) column kept at 30°C with an isocratic flow at a flow rate of 1.0 ml/min. The detector temperature was 30°C, the retention time of PVA was around 1.0 min and the total run time was 5 minutes. Conclusion: The proposed method showed linearity, accuracy, precision, specificity, robustness, solution stability, and system suitability results within the acceptance criteria.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (03) ◽  
pp. 39-45
Author(s):  
A Sherje ◽  
A. Sonalkar ◽  

A reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of olmesartan medoxomil (OLME) and chlorthalidone (CHLOR) in tablet dosage form. The analysis was performed on Inertsil ODS C18 (250 x 4.6 mm, 5 μ) using KH2PO4 phosphate buffer (pH) and acetonitrile as mobile phase in the proportion of 60: 40 v/v at flow rate of 1.0 mL/min. Detection of drugs was carried out in isocratic mode using UV detector at 275 nm. The retention time of OLME and CHLOR was 13.9 ± 0.1 min. and 4.4 ± 0.5 min., respectively and the total run time was 20 min. The method was validated according to the requirements of the United States Pharmacopeia. The percentage recoveries was found to be in the range of 98.9 - 100.7%. The method was successfully applied to the assay of OLME and CHLOR in tablet dosage form.


2010 ◽  
Vol 7 (s1) ◽  
pp. S299-S313 ◽  
Author(s):  
P. Shetti ◽  
A. Venkatachalam

A new, simple, precise, rapid, selective and stability indicating reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for simultaneous quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and chlorpromazine hydrochloride from combined tablet formulation. The method is based on reverse-phase using C-18 (250×4.6) mm, 5 μm particle size column. The separation is achieved using isocratic elution by methanol and ammonium acetate buffer (1% w/v, pH 6.5) in the ratio of 85:15 v/v, pumped at flow rate 1.0 mL/min and UV detection at 215 nm. The column is maintained at 30 °C through out the analysis. This method gives baseline resolution. The total run time is 15 min. Stability indicating capability is established buy forced degradation experiment. The method is validated for specificity, accuracy, precision and linearity as per International conference of harmonisation (ICH). The method is accurate and linear for quantification of trihexyphenidyl hydrochloride, trifluoperazine hydrochloride and Chlorpromazine hydrochloride between 5 - 15 μg/mL, 12.5- 37.5 μg/mL and 62.5 - 187.5 μg/mL respectively.


Author(s):  
D. Chinababu

Aim: The objective of the study was simplest, accurate, precise and robust reversed phase high performance liquid chromatographic (RP-HPLC) method was developed for the estimation of Velpatasvir (VEL) and Sofosbuvir (SOF) in the bulk and its tablet dosage form. Study Design: The Quantitative and Qualitative estimation and designed forced degradation study of Velpatasvir & Sofosbuvir by RP-HPLC. Place and Duration of Study: The study was carried at Santhiram College of Pharmacy and time taken 4 months. Method: The method was attained by used Waters( 5µm, C18 250 x 4.6 mm) column with mobile phase consists of  0.5 mM disodium hydrogen phosphate buffer pH adjusted to 6.5, with Orthophosphoric acid and Methanol in the ratio of 78:22 v/v, a flow rate of 1.0 mL/min and ultraviolet detection at 285 nm. Results: The method was validated as per ICH guidelines with different parameters, the mean retention times of VEL and SOF were found to be 2.8 & 4.7 min respectively. The resolution between VEL and SOF was found to be 10.66. The Correlation coefficients for calibration curves within the detection range of 32.5 - 97.5 and 125 - 375 µg/mL were 0.999 for VEL and SOF respectively. The LOD and LOQ for VEL and SOF were found to be 0.0068-0.029 µg/mL and 0.104-0.342 µg/mL respectively. Conclusion: The results were indicated that the developed method was used for the routine analysis of VEL & SOF combined form in bulk and its commercial formulation. To the best of our knowledge, there was no method of RP-HPLC for the determination of VEL alone or in combination with SOF molecule.


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 34-41
Author(s):  
S. K Kondila ◽  
◽  
K Sujana ◽  
A Prameela Rani

The aim of the present work was to develop and validate an accurate, precise, simple, and efficient stability indicating Reversed phase High Performance Liquid Chromatography method for determination of an abrisentan and its process impurities in bulk and pharmaceutical dosage forms. The drug substance was subjected to stress conditions such as hydrolysis (acid and base), oxidation, photolysis and thermal degradation as per International Conference on Harmonization guidelines to study the stability-indicating profile of drug. Significant degradation was observed during acid hydrolysis and peroxide degradation. The chromatographic conditions were optimized using an impurity-spiked solution and samples generated from forced degradation studies. The method was developed using Agilent XDB-C18 (150×4.5mm, 5μ) column and 10mM NH4OAc (pH-5.2 adjusted with acetic acid): ACN as the mobile phase with gradient programme at a flow rate of 1 mL/min. effluents were monitored at 289 nm. The retention times were found as 25.945 min for IMP-1, 24.685 min for IMP-2, 23.83 min for IMP-3, 10.53 min for AMB, 5011 min for IMP-4 and 3.48 min for IMP-5. The mean recovery values were found to be 98.52-100.44% for AMD and its impurities. The degradation rate of AMB in acid, base, peroxide (oxidative) thermal and photolytic degradation processes was found in range 7-22%. The developed analytical method has been validated for specificity, linearity, precision, accuracy, and robustness which were within the acceptance limit according to ICH guidelines. The developed method was successfully employed for routine quality control and stability analysis of AMB in pharmaceutical dosage forms.


2021 ◽  
Vol 57 (16) ◽  
pp. 2093-2096
Author(s):  
Liangyou Lin ◽  
Camilla Lian ◽  
Timothy W. Jones ◽  
Robert D. Bennett ◽  
Blago Mihaylov ◽  
...  

We developed a high-performance hole transport material based on transition metal complexes for perovskite solar cells, which exhibits excellent photostability.


2020 ◽  
Vol 8 (1) ◽  
pp. 15-20
Author(s):  
Yuni Retnaningtyas ◽  
Nia Kristiningrum ◽  
Hidayah Dwi Renggani ◽  
Indah Purnama Sary

The stability indication of Reversed Phase-High Performance Liquid Chromatography (RP-HPLC) method was validated for quantitative determination of mangiferin on three species mango leaves (Mangifera odorata Griff, Mangifera foetida Lour, and Mangifera indica L.). The samples were extracted by maseration method using methanol and concentrated using rotary evaporator. The method carried out on stationary phase a purospher RP-18 endcapped (25 cm × 4.6 mm i.d., 5 µm) column with a mobile phase consisting of methanol: phosphoric acid 0.1% (v/v) (31:69); flow rate:0.8 mL/min; solvent methanol, detection was carried out at 258 nm. The analytical  performace this measurement is good with the value of linearity (r2=0.998), precision (%RSD=0.649%), and accuration (10.67%). The forced degradation studies were carried out according to the International Conference on Harmonization (ICH) guidelines. The results indicating that the complete separation between degradation products and mangiferin peak occured. The degradation limit of mangiferin 5–20% (according to the guideline of ICH) except in basic condition (100%). The method was succesful applied to determine of the mangiferin in  pakel (Mangifera foetida), kweni (Mangifera indica) and kopyor (Mangifera odorata) extract. The mangiferin content was obtained are pakel (9.95%), kopyor (7.40%) and kweni (Mangifera odorata) (2.49%) respectively.


2015 ◽  
Vol 39 (3) ◽  
pp. 1587-1591 ◽  
Author(s):  
Daniel Mendoza-Espinosa ◽  
Rodrigo González-Olvera ◽  
Cecilia Osornio ◽  
Guillermo E. Negrón-Silva ◽  
Rosa Santillan

A series of O- and S-functionalized triazolium salts display high performance in the Baylis–Hillman addition and allow the one-pot formation of MIC-transition metal complexes.


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