Current Issue : July-September Volume : 2025 Issue Number : 3 Articles : 8 Articles
The present work aims to establish a simple, precise and rapid spectrophotometric method for quantifying ascorbic acid in active pharmaceutical ingredients. In this, work is carried out to estimate Ascorbic acid bulk by utilizing an Area under Curve (AUC) method using UV – UV-visible spectrophotometry. The study is designed to validate the developed methods as per ICH guidelines. For this purpose, the wavelength range between 200-400 nm was selected. Distilled water was used as a solvent throughout the work. Linearity was obtained in the concentration range of 2 to 10 µg/ml (r2 =0.991) for the method. The developed method was found to be simple, linear, accurate, precise and highly sensitive and can be used for routine quality control analysis for spectrophotometric estimation of active pharmaceutical ingredients....
Imipenem (IMP) and Cilastatin (CILA) are co-formulated β-lactam antibiotics extensively used in the management of severe bacterial infections, requiring reliable analytical methods for simultaneous estimation to ensure quality control and regulatory compliance. A simple, accurate and reproducible reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the concurrent quantification of IMP and CILA in bulk and pharmaceutical dosage forms in accordance with ICH Q2(R1) guidelines. Chromatographic separation was performed on a Zodiac Sil RP-C18 column (250 × 4.6 mm, 3.0 µm) using a mobile phase of methanol and phosphate buffer (pH 3.0) in a 70:30 (v/v) ratio at a flow rate of 1.0 mL/min, with UV detection at 240 nm and an injection volume of 10 µL. IMP and CILA were well resolved with retention times of 2.45 and 3.19 min, respectively and a resolution greater than 3.0. The method exhibited excellent linearity in the ranges of 50–250 µg/mL for IMP and 5–25 µg/mL for CILA with correlation coefficients (r²) of 0.999 for both drugs. Accuracy studies demonstrated mean recoveries of 99.54% for IMP and 100.75% for CILA, while intra- and inter-day precision values were within 2% RSD. The method demonstrated high sensitivity with LOD/LOQ values of 2.16/6.62 µg/mL for IMP and 0.037/0.11 µg/mL for CILA. Robustness was confirmed under deliberate variations in flow rate and mobile phase composition. The proposed method is rapid, sensitive and reliable, making it highly suitable for routine quality control and stability testing in pharmaceutical industries....
A stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous estimation of Telmisartan (TEL) and Azelnidipine (AZE) in fixed-dose combination formulations. Chromatographic separation was achieved on an Inertsil ODS C18 column (250 × 4.6 mm, 5 μm) using phosphate buffer (pH 3.0) and acetonitrile in a 70:30 (v/v) ratio as the mobile phase at a flow rate of 1.0 mL/min. Detection was carried out at 225 nm with a 20 μL injection volume. The method was validated in accordance with ICH Q2 (R1) guidelines and met all criteria for system suitability, linearity, precision, accuracy, sensitivity, robustness and stability-indicating capability. TEL and AZE eluted at 2.798 and 3.587 minutes, respectively, with resolution values greater than 2.0 and tailing factors not exceeding 1.2. Calibration curves were linear over the ranges of 100–500 μg/mL for TEL and 20–100 μg/mL for AZE, both showing correlation coefficients of 0.999. Accuracy studies demonstrated recoveries between 98.5% and 100.1%, while precision results confirmed reproducibility with %RSD below 2%. The method exhibited excellent sensitivity, with LOD and LOQ values of 3.72 and 7.40 µg/mL for TEL and 0.0242 and 0.0202 µg/mL for AZE, respectively. Forced degradation under acidic, alkaline, oxidative, thermal and photolytic conditions confirmed that degradation products were well resolved from the analyte peaks, demonstrating the stability-indicating power of the method. The proposed RP-HPLC method is simple, accurate, precise and robust, making it highly suitable for routine quality control, stability testing and regulatory applications of TEL and AZE in bulk and pharmaceutical dosage forms....
Vitamin A (retinylpalmitate) and E (α-tocopherol) are essential fat-soluble micronutrients that play critical roles in maintaining human health and their accurate quantification in food matrices such as eggs is vital for nutritional assessment, quality control and regulatory compliance. A simple, precise and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous estimation of Vitamins A and E in egg yolk. Chromatographic separation was achieved on an RP-C18 column (250 × 4.6 mm, 10 µm) using methanol and acetonitrile (30:70, v/v) as the mobile phase under isocratic conditions at a flow rate of 1.0 mL/min. Detection was performed at 264 nm for Vitamin E and 325–395 nm for Vitamin A. Sample preparation involved saponification with ethanolic potassium hydroxide, followed by liquid–liquid extraction and reconstitution in hexane. The method provided baseline resolution of Vitamin E (retention time ≈ 7 min) and Vitamin A (retention time ≈ 9 min) without interference from matrix components, confirming specificity. Linearity was observed across the ranges of 0.1–100 ppm for Vitamin E (r² = 0.999) and 0.1–1.3 ppm for Vitamin A (r² = 0.997). Precision studies showed excellent repeatability with %RSD values below 1%, while accuracy was confirmed with mean recoveries of 99.8% for Vitamin E and 100.1% for Vitamin A. Sensitivity was established by low LOD and LOQ values and robustness testing confirmed method reliability under minor variations in chromatographic conditions. This validated RP-HPLC method is rapid, accurate and reproducible, making it highly suitable for routine food quality control, nutritional evaluation and regulatory applications....
Nitrosamine impurities, including N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA), are classified as genotoxic and carcinogenic. Their occurrence in pharmaceuticals, even at trace levels, necessitates sensitive analytical methods. Palaveratone, a steroidal active pharmaceutical ingredient, requires rigorous monitoring for these impurities. This study aimed to develop and validate a simple, reliable and sensitive RP-HPLC method for the quantification of NDMA and NDEA in palaveratone, following ICH Q2(R1) and ICH M7(R1) guidelines. Chromatographic separation was performed on a Platisil C18 column (250 × 4.6 mm, 5 µm) with an isocratic mobile phase of potassium dihydrogen phosphate buffer and acetonitrile (10:90 v/v). The flow rate was 1.0 mL/min, detection wavelength 296 nm and injection volume 20 µL. The method was validated for specificity, linearity, precision, accuracy, detection limit (DL) and quantitation limit (QL). NDMA and NDEA were well resolved without interference. The DL and QL were 0.035 ppm and 0.093 ppm, respectively. Linearity was excellent (R² = 0.999), recoveries ranged from 98.2–115.2% and precision studies yielded %RSD values <6%. Intermediate precision met the cumulative acceptance limit of ≤20.0. The validated method was found sensitive, accurate and reproducible, making it suitable for routine quality control and regulatory compliance of nitrosamine impurities in palaveratone....
An analytical mapout was framed for the establishment of sofosbuvir in bulk and tablet dosage form. The high performance thin layer chromatographic technique was attempted; the stationary phase used for this investigation is silica gel 60 F254 HPTLC plate. The ethyl acetate: methanol: Toluene in the volume ratio of 6.0:2:0:2.0 was the mobile phase. The Rf value was optimized as 0.42. The determination was performed at 260 nm. The validations were stepped for the various parameters such as linearity, accuracy, precision and specificity. The statistical analysis has been demonstrated for the confirmation and assurance of accuracy and reproducibility. The linearity range was 100 to 500 ng/spot. The limit of detection and limit of quantitation for sofosbuvir were 20 and 60 ng/spot respectively. The novel design can be successfully applied for the analytical establishment of Sofosbuvir in the tablet dosage form....
Dasatinib and Lenvatinib are tyrosine kinase inhibitors widely prescribed for hematological malignancies and solid tumors. Their simultaneous estimation in pharmaceutical dosage forms is critical for quality control, therapeutic safety and regulatory compliance, especially when used in combination regimens. Chromatographic separation was achieved on a Shim-pack C18 column (150 × 4.6 mm, 5 µm) using an isocratic mobile phase of phosphate buffer (0.05 M, pH 3.0) and acetonitrile (35:65, v/v) at a flow rate of 1.0 mL/min. Detection was performed at 265 nm with a 10 µL injection volume. Validation parameters included system suitability, specificity, linearity, accuracy, precision, robustness and sensitivity. Dasatinib and Lenvatinib were eluted at 2.4 and 3.5 minutes, respectively, with sharp and well-resolved peaks. The method demonstrated excellent linearity (R² > 0.9999), recoveries of 99–101% and %RSD < 2%. LODs were 0.082 µg/mL and 1.13 µg/mL, respectively. Assay results of marketed formulations confirmed drug content within 99–101% of label claims. The validated RP-HPLC method is rapid, accurate, precise and robust, making it suitable for routine quality control, stability testing and regulatory applications....
Cefpodoxime proxetil, a third-generation cephalosporin and ambroxol hydrochloride, a mucolytic agent, are frequently co-formulated for the treatment of respiratory tract infections, necessitating reliable analytical methods for simultaneous estimation in pharmaceutical dosage forms. A robust and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the quantification of these drugs in combined formulations in accordance with ICH Q2(R1) guidelines. Chromatographic separation was achieved using a Phenomenex C18 column with a mobile phase of methanol and phosphate buffer (pH 4.5) in a 70:30 (v/v) ratio, at a flow rate of 1.0 mL/min, with detection carried out at 254 nm. Validation parameters assessed included specificity, linearity, precision, accuracy, sensitivity, robustness and system suitability. The method demonstrated excellent linearity in the concentration ranges of 50–150 µg/mL for cefpodoxime proxetil and 30–90 µg/mL for ambroxol hydrochloride, with correlation coefficients (R²) greater than 0.999 for both analytes. Accuracy studies yielded mean recoveries within 98–102%, while precision results confirmed reproducibility with %RSD values below 2%. Limits of detection and quantitation confirmed the sensitivity of the method and deliberate variations in chromatographic conditions verified robustness. All system suitability parameters met acceptance criteria, further establishing the reliability of the method. The proposed RP-HPLC method is simple, rapid, precise, accurate and stability-indicating, making it highly suitable for routine quality control, batch release testing and regulatory submissions of cefpodoxime proxetil and ambroxol hydrochloride in combined pharmaceutical dosage forms....
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