1. | A STUDY OF METHOD DEVELOPMENT, VALIDATION, AND
FORCED DEGRADATION FOR SIMULTANEOUS
QUANTIFICATION OF NIVOLUMAB AND RELATLIMAB IN
PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD |
| Aswin Kumar N1, Chitra M2*, Vijayamithraj R, Senthil Kumar N |
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To gain some additional advantages over other methods already created for this combination, a rapid and stability-indicating
reversed phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous quantification
of Nivolumab and Relatlimab in their combined dosage form. According to USP guidelines for accuracy, precision,
specificity, linearity, solution stability, robustness, sensitivity, and system appropriateness, the method was validated.
According to the International Conference on Harmonisation (ICH), the forced degradation study was verified. According to
the International Conference on Harmonisation (ICH), the forced degradation study was verified. For this, an isocratic
condition of mobile phase was maintained on RP C18 (octadecylsilane (ODS), 150 4.6 mm, 5 m, Phenomenex Inc.) column
at room temperature. The mobile phase consisted of phosphate buffer (pH 6.8) and acetonitrile at a ratio of 65:35, v/v, With
correlation coefficient (R2) values of 0.999 and 1.0 for Nivolumab and Relatlimab, respectively, the method demonstrated
excellent linear response and was within the correlation coefficient's range (R2? 0.995). Two medication’s percent recoveries
fell within the acceptable range of (99.60-99.82.%).The novel method's intra- and inter-day precision assessments showed
that the relative standard deviation (%RSD) was less than the 2.0 maximum permitted limit. According to ICH guidelines, the
drug product was forced to degrade in order to determine its stability-indicating ability and learn more about the degradation
pathways, degradation products, and how the quality of a drug substance and drug product varies over time under different
stressful conditions. Relatlimab degradation was within the acceptable range (5-20%, per ICH guidelines), however
Nivolumab demonstrated a 20% degradation in oxidation and basic condition
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2. | REVIEW ON COMPARISON BETWEEN HPLC AND UPLC
METHOD IN PHARMACEUTICAL ANALYSIS |
| Malathi S, Leelavathi A |
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Pharmaceutical analysis plays a crucial role in ensuring the safety, efficacy, and quality of drug products. High-performance
liquid chromatography (HPLC) has been the cornerstone technique for many years. However, in recent years, ultrahighperformance liquid chromatography (UPLC) has emerged as a promising alternative. This review aims to provide a
comprehensive comparison between HPLC and UPLC methods in pharmaceutical analysis, highlighting their advantages,
limitations, and application considerations. The review begins by discussing the fundamental principles and operating
parameters of both HPLC and UPLC systems. It elaborates on the differences in column particle size, column dimensions,
and system pressures, which significantly impact the separation efficiency and analysis time. Various practical aspects, such
as instrument cost, method development, and compatibility with existing HPLC methods, are also addressed. Next, the
review evaluates the analytical performance of HPLC and UPLC methods, including resolution, sensitivity, linearity, and
precision. The enhanced resolution and sensitivity offered by UPLC are explored, along with its ability to achieve shorter
analysis times and improved peak shapes. Additionally, the impact of different sample matrices and analyte properties on
method selection is discussed, highlighting scenarios where HPLC or UPLC may be more suitable.The limitations and
challenges associated with both techniques are critically analyzed, covering aspects such as column lifetime, system
robustness, and method transferability. Practical guidelines for method development and optimization are provided to assist
analysts in selecting the most appropriate technique based on their specific requirements. In summary, this review offers a
comprehensive comparison between HPLC and UPLC methods in pharmaceutical analysis. It provides valuable insights into
the advantages and limitations of each technique, assisting researchers and analysts in making informed decisions regarding
method selection, development, and optimization in the field of pharmaceutical analysis
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3. | 2D-QSAR AND IN SILICO PHARMACOLOGICAL EVALUATION
OF SOME NOVEL ?-CARBOLINE ANALOGUES |
| Mohammad Yunus*, Om Prakash Agrawal |
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A series of 51 compounds [N-(substituted-benzylidene)- -carboline-3-carbohydrazide derivatives having significant
inhibitory activity against cancer cell lines was selected and the presented biological activity (in micromolar concentration) of
those compounds were conveniently converted into Log (1/IC50) values (molar) for carrying out QSAR analysis against anticancer activities using Chemoffice Ultra version 7.0.1, from Cambridge software corporation. The values of related
parameters of all the molecules were calculated after effective energy minimization through MM2, MOPAC force fields
provided by Chem3D Ultra 7.0.1. The best QSAR model obtained was taken into consideration on the basis of high Q2 value,
which reveals that in order to increase the biological activity, the properties like Log P, and Charge-dipole energy should be
increased, whereas Bending energy which is showing a negative value in the equation should be decreased. Thus, it is
concluded that the biological activity will be increased if substituents that bring about changes in the molecule as mentioned
above are attached to it. As per the given QSAR data, a new series of 1-substituted ?-carboline derivatives (1a1k) were
synthesized having increased LogP value. These title compounds containing seven different substituents at C-1 were screened
for their invitro anti-cancer and Anti-microbial activity. Most of the test compounds were found to exhibit significant anticancer activity. Among the substituents at C-1, isopropyl substituent showed maximum potency, while n-propyl substituent
showed equipotent activity remaining substituents exhibited least activity when compare to other substituents. The order of
activity at C-1 is as understood by QSAR factor (Compound 1e) was found to be the most active agent which showed highest
percentage of cell inhibition against all the cancer cell lines in the minimum concentration, which have isopropyl group at the
1st position in the ?-carboline nucleus. Hence this molecule can be selected as a lead molecule of the present study for further
exploitation
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4. | DEVELOPMENT AND VALIDATION OF A HPLC METHOD FOR
THE DETERMINATION OF METFORMIN HYDROCHLORIDE,
NATEGLINIDE AND PIOGLITAZONE HYDROCHLORIDE IN
MULTI COMPONENT FORMULATION |
| Prashant Dubey & Om Prakash Agrawal |
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A simple, rapid, and precise reverse-phase high-performance liquid chromatographic method for simultaneous analysis of
Metformin hydrochloride, Nateglinide, and Pioglitazone hydrochloride in a tablet dosage form has been developed and
validated. Chromatography was performed on a 25 cm × 4.6 mm i.d., 5-mm particle, C18 column with 85:15 (v/v) methanol:
20 mM potassium dihydrogen phosphate buffer as mobile phase at a flow rate of 1.2 ml/min. UVdetection at 227 nm;
Metformin hydrochloride, Nateglinide, and Pioglitazone hydrochloride were eluted with retention times of 2.15, 3.787, and
4.57 min, respectively. The method was validated in accordance with ICH guidelines. Validation revealed the method is
specific, rapid, accurate, precise, reliable, and reproducible. Calibration plots were linear over the concentration ranges 50-
250 mg/ml for Metformin hydrochloride, 3.0-15.0 mg/ml for Nateglinide, and 2-10 mg/ml for Pioglitazone hydrochloride.
Limits of detection were 0.03, 0.22, and 0.008 mg/ml and limits of quantification were 0.09, 0.67, and 0.02 mg/ml for
Metformin hydrochloride, Nateglinide, and Pioglitazone hydrochloride, respectively. The high recovery and low coefficients
of variation confirm the suitability of the method for simultaneous analysis of the three drugs in tablets. Statistical analysis
proves that the method is suitable for the analysis of Metformin hydrochloride, Nateglinide, and Pioglitazone hydrochloride
as a bulk drug and in pharmaceutical formulation without any interference from the excipients. It may be extended to study
the degradation kinetics of three drugs and also for its estimation in plasma and other biological fluids
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5. | ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR
THE ESTIMATION OF POSACONAZOLE IN PHARMACEUTICAL
FORMULATIONS – A REVIEW |
| Saravanan C*, Surya D, Surya prakash C.T, Swetha S, Syed Sameer Basha G,
Tamilarasi Y |
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Posaconazole marketed under the trade name Noxafil among others, is a medication used to treat serious fungal infection.
Posaconazole, a broad-spectrum triazole antifungal agent, is approved for the preventionof invasive aspergillosis and
candidiasis in addition to the treatment of oropharyngeal candidiasis. There is evidence of efficacy in the treatment and
prevention of rarer, more difficult-to- treat fungal infections. Posaconazole oral suspension solution has shown limitations
with respect to fasting state absorption, elevated gastrointestinal ph and increased motility. The newly approved delayedrelease oral tablet and intravenous solution formulation provide an attractive treatment option by reducing interpatient
variability and providing flexibility in critically ill patients. On the basis of clinical experience and further clinical studies,
posaconazole was found to be a valuable pharmaceutical agent for the treatment of life-threatening fungal infection. This
review will examine the development history of posaconazole and highlight the most recent advances
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6. | PHYTO-CHEMICAL FOR RESPIRATORY HEALTH: A
COMPREHENSIVE REVIEW ON THEIR THERAPEUTIC
APPLICATIONS IN LUNG DISORDERS |
| Indhumathy P |
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This comprehensive review examines the therapeutic applications of phyto-constituents in respiratory health and their
potential in managing lung disorders. Phyto-constituents are naturally occurring chemical compounds found in plants, known
for their diverse properties such as anti-inflammatory, antioxidant, antimicrobial, immune-modulating, bronchodilatory, and
mucolytic effects. By targeting key mechanisms involved in respiratory ailments, these natural compounds offer promising
avenues for alleviating symptoms, improving lung function, and enhancing overall respiratory well-being. The review
emphasizes the importance of understanding the mechanisms of action, appropriate dosages, and safety considerations of
phyto-constituents. Future research directions, including the identification of novel phyto-constituents, conducting clinical
trials, and exploring synergistic combinations, are also discussed. Harnessing the therapeutic potential of phyto-constituents
can contribute to the development of natural and complementary approaches in respiratory health management, benefiting
individuals with lung disorders
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7. | DETERMINATION AND ESTIMATION OF AMBROXOL HCL,
GUAIPHENESIN BY USING UV- VISIBLE
SPECTROPHOTOMETERIC METHOD |
| V. Garamsandh Gandhi*, R. Sivakumar, A. Mouli, K. Praveen, S. Satheesh,
N. Veerasundaramoorthy |
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In this project we are going to analyse the four simple, rapid, accurate, precise, reliable and economical
spectrophotometric methods have been proposed for simultaneous determination of Ambroxol, guaiphenesin in pure and
pharmaceutical formulations without any prior separation or purification step. The methods are first derivative zero crossing
spectrophotometry, simultaneous equation, derivative ratio spectra zero crossing and double divisor ratio spectra derivative
method. Developed methods show best results in terms of linearity, adsorption for standard laboratory mixtures of pure drugs
and marketed formulations. Common excipients and additives did not interfere in determinations of these APIs. The results
obtained by the proposed methods have been statistically compared by means of student t-test
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