Bulk Drug Research Articles

Separation and quantification of organic‐related impurities of beta‐adrenergic receptor blocking agent propranolol in pharmaceutical solid dosage forms: Impurity profiling using stability‐indicating HPLC method

AbstractPropranolol hydrochloride (PPH) is a medication of beta‐adrenergic receptors. It is used to treat pediatric hemangiomas that are growing and need systemic therapy. A reversed‐phase high‐performance liquid chromatography (HPLC) was made to separate and estimate the amounts of ten known organic impurities of propranolol in bulk drugs, tablets, and capsule dosage forms. The chromatographic separation was achieved on a C18 column (100 × 4.6 mm, 2.7 μm) using a binary gradient mixture of pH 2.3 phosphate buffer and organic modifiers of acetonitrile, methanol, and isopropyl alcohol as the mobile phase. The stability‐indicating character of the proposed method was proven using stress testing study. The test method was validated for specificity, limit of detection, limit of quantitation, linearity, precision, accuracy, and robustness. For the propranolol and its ten organic impurities, the limit of quantitation, linearity, and recoveries were found in a range of 0.0123–0.4266 μg/mL (R2 > 0.9982) and 89.2–98.9%, respectively. The proposed liquid chromatography method is found to be highly suitable for impurity profiling of propranolol in bulk drugs and pharmaceutical formulations (tablets and capsules).

Development of stability-indicating HPLC method for quantification of pharmacopeia impurities of Zuclopenthixol and characterization of its stress degradation products by LCMS/MS

BackgroundThe present study focused to develop a simple and sensitive HPLC method for resolution and estimation process-related impurities of zuclopenthixol and further assessment of forced degradation behavior of zuclopenthixol.ResultsThe chromatographic separation of drug substance, process-related impurities and its degradation products (DPs) was achieved on KNAUER C18 (250 mm × 4.6 mm, 5µ id) column at that was maintained at 35 °C temperature using 0.1 M sodium acetate buffer at pH 4.3 and methanol in 20:80 (v/v) as mobile phase A, 0.1% formic acid and acetonitrile in 75:25 (v/v) as mobile phase B. Equal volume of mobile phase A and B was pumped in isocratic elution at 0.8 mL/min. Detection wavelength was selected as 257 nm. In the proposed conditions, zuclopenthixol is identified at 6.91 and 1.91 min and 2.89 min, respectively, for impurity B and A min with acceptable system suitability and specificity. The method produces LOD at 0.009 for impurities with calibration range of 30–180 µg/mL for zuclopenthixol and 0.03–0.18 µg/mL for impurities. The other validation parameters were notices to be with in the acceptable levels for zuclopenthixol and its impurities. The drug was exposed to different stressed conditions (acid, base, peroxide, thermal and UV light) according to ICH Q1A (R2) guidelines. The DPs formed during the stress study were identified and characterized by LCMS/MS in ESI positive mode.ConclusionThe analysis involved a comparison of collision-induced dissociation mass spectrometry data between the degradation products and zuclopenthixol. As a result, potential structures for six degradation compounds were suggested. The results from additional validation studies were similarly pleasing and demonstrated their suitability for the routine analysis of zuclopenthixol and its associated impurities in both bulk drug and pharmaceutical dosage forms. Additionally, these findings can be extended to assess the mechanism of stress degradation in zuclopenthixol.

Eco-friendly micellar HPLC approach for simultaneous estimation of combination therapy for hidradenitis suppurativa: Applications to spiked human plasma and different dosage forms.

This study introduces a new method for analyzing rifampicin, moxifloxacin, and metronidazole using a green micellar High Performance Liquid Chromatography-Ultraviolet method in bulk drugs, different commercial formulations, and spiked human plasma. The combined therapy of these three broad-spectrum antibiotics is used to cure refractory hidradenitis suppurativa (HS), an inflammatory condition affecting the skin. The sustainable separation was attained on a reversed-phase C18 Kinetex® column maintained at ambient temperature in less than 5 min. The mobile phase comprises 0.1 M sodium dodecyl sulfate (SDS) in water, pH 3.5, adjusted using o-phosphoric acid, and 10% n-butanol. The flow rate was 1 mL/min, with 10 μL injection volume and UV detection at 230 nm. The impact of three key significant variables, SDS concentration, n-butanol percentage, and the mobile phase pH, on suitability parameters was studied. ICH and FDA guidelines were committed to when validating the technique. The results showed linear calibration graphs with high precision and accuracy, in both pure and spiked plasma. The method is efficient, easy to use, and has a high sample throughput, making it suitable for routine analysis in the quality control department and therapeutic monitoring. It is also evaluated as a green-and-white substitute for traditional reported methods.

Optimization of Stability-Indicating HPLC Method for Analyzing Process Related Impurities of Penfluridol and Structural Elucidation of Stress Degradation Products by LCMS/MSucidation of Stress Degradation Products by LCMS/MS

This study focused on the development of a simple and sensitive HPLC method for resolution and quantification of process-related impurities of penfluridol and further assessment of forced degradation behavior of penfluridol. The chromatographic separation was achieved on XTerra™ C18 (250×4.6 mm, 5.0μm) column and UV detection at 245nm. The mobile phase comprises of methanol and tetrahydrofuran in 55:45 (v/v) as solvent A and acetonitrile and tetrahydrofuran in 80:20 (v/v) as solvent B. The 60:40 (v/v) composition of solvent A and B were pumped isocratically at 1.0mL/min. In the proposed conditions, the retention time identified as 5.29 min for penfluridol, 4.51 min, 9.95 min and 7.64 min respectively for impurity 1, 2 and 3 with acceptable system suitability. The method produces sensitive detection limit of 0.008μg/mL for impurity 1, 2 and 0.004 μg/mL for impurity 3 with calibration range of 25-150 μg/mL for penfluridol and 0.025-0.150 μg/mL for impurities. The drug was exposed to different stressed conditions (acid, base, peroxide, thermal and UV light) according to ICH Q1A (R2) guidelines. The Degradation Products (DPs) formed during the stress study was characterized by LCMS/MS in ESI positive mode and the possible structures of five DPs with possible degradation pathways were proposed. The outcomes of other validation studies were likewise satisfactory and proven adequate for regular analysis of penfluridol and its process-related impurities in bulk drug and pharmaceutical dosage forms and can also applicable for evaluation of stress degradation mechanism of penfluridol.

Methods Development and Validation for the Estimation of Pioglitazone HCl in Bulk and Formulations by UV Spectroscopy and FTIR

The use of spectroscopic analysis, particularly UV spectrophotometer, is a simple and essential technique for bulk drug estimation, formulation studies, and compatibility assessments of drugs with various excipients. In the pharmaceutical industry, various analytical instruments, including Fourier transform infrared spectroscopy (FTIR), are employed for investigating drug-excipient interactions that can impact the stability of active pharmaceutical ingredients. This study aimed to develop a UV spectrophotometric method for the analysis of Pioglitazone hydrochloride in phosphate buffer (pH 7.4) and methanolic solution, assessing its linearity and compliance with Beer's Law. Furthermore, we aimed to use FTIR to characterize potential interactions between Pioglitazone and common pharmaceutical excipients, such as Guar Gum, Chitosan, and Sodium Alginate. Standard solutions of Pioglitazone were prepared in phosphate buffer (pH 7.4) and methanol. UV spectrophotometer was conducted to determine the maximum absorption wavelength. Calibration curves were constructed to evaluate linearity and adherence to Beer's Law. FTIR analyses were performed to investigate drug-excipient interactions by examining the functional groups. In phosphate buffer (pH 7.4), the maximum absorption wavelength for Pioglitazone hydrochloride was 268 nm. The calibration curve for Pioglitazone in phosphate buffer (pH 7.4) demonstrated linearity in the concentration range of 1–20 µg/ml, with a correlation coefficient of 0.998. In methanol, the maximum absorption wavelength for Pioglitazone hydrochloride was found to be 272 nm. The calibration curve in methanol exhibited linearity in the range of 1–20 µg/ml, with a correlation coefficient of 0.999. FTIR analysis revealed potential drug-excipient interactions, particularly in the case of Guar Gum, Chitosan, and Sodium Alginate, suggesting the formation of stable hydrogen bonds. The developed UV spectrophotometric method for Pioglitazone analysis is a reliable, cost-effective, and reproducible approach, making it a valuable tool for drug development and quality control. Additionally, the FTIR characterization confirmed interactions between Pioglitazone and common pharmaceutical excipients, enhancing our understanding of formulation compatibility.

Development and Validation of an Innovative Stability Indicating Method Using UVSpectroscopy Techniques for Ritonavir in Bulk Drug and Pharmaceutical Dosage Forms

Ritonavir is a protease inhibitor used to treat HIV/AIDS. It is seldom employed for its antiviral activity but instead as a booster for other protease inhibitors. Our study's significant objective is to develop a new, simple, accurate, precise, and reproducible UV spectrophotometric approach for investigation by apotheosis to analyze ritonavir. Three alternative simple, accurate, and precise UV spectrophotometric techniques-the, zero-order (method A), first-order (method B), and the area under the curve (method C) spectrophotometric methods have been established for the measurement of ritonavir in bulk and pharmaceutical dosage. The drug was dissolved in ethanol, and then 0.063 M Phosphate buffer solution (pH 7.0), and the observed λmax are 271 nm for the zero-order spectrophotometric method (method A), 258 nm for the first-order spectrophotometric method, 260–281 nm for the area under the curve spectrophotometric method (method C). Under the optimum conditions, linear relationships with good correlation coefficients 0.9994–0.9999 were found between the reading and the corresponding concentration of the drug in the range of 10-50 μg/ml. The proposed methods can detect the analyte in the lower limits of 0.24 to 0.38 μg/ml. The precision of the methods was satisfactory, and the percentage relative standard deviation values did not exceed 2%. The proposed methods were successfully applied to the analysis of ritonavir in its bulk and commercial formulations with good repeatability and reproducibility; the label claim percentages ranged from 99.56 to 99.64 ± (0.34-0.63) % w/v. The research findings of the current approach were shown to be more accurate and trustworthy for ritonavir in pharmaceutical dosage forms and bulk pharmaceuticals compared to those previously reported by the spectrophotometric approaches. The proposed techniques can be used for routine inspections without causing any interference from excipients or other substances because of the quick and repeatable analysis.

Computational analysis of hybrid grey wolf and particle swarm optimization for water level control in coupled tank

<p><span>Water level control at a precise set point is a major concern in process control systems such as bulk drug production industries. Loss in production at the initial stage is observed until the water level reaches desired level. Pharmaceutical industries can however be benefited if they could maintain the precise water level control at the initial stage of production with the help of the performance optimization using various techniques. To achieve optimized value of the selected performance index, a hybrid of particle swarm optimization (PSO) and grey wolf optimization (GWO) is found to provide the desired performance in the best possible manner. The mathematical model of the coupled tanks is first developed using the state space analysis which can then be converted to transfer function form so as to accomplish the simulation. In this paper, integral square error (ISE) is selected as the performance index for the minimization to improve overall performance of the system. <span>Observations from the hybrid GWO-PSO optimization articulate that overshoot and settling time can be improved as per the industry needs. Performance evaluation of different optimization techniques is discussed in this paper.</span></span></p>

Spectrophotometric Method Development for Estimation of Multicomponent Antidiabetic Drugs in Bulk and Solid Dosage Form

Abstract: The aim of the present study was the development and validation of a simple, precise and accurate UVspectrophotometric method for the estimation of metformin (MET), voglibose (VOG) and pioglitazone (PIO) in bulk and tablet dosage form using methAanol as solvent. The method was proposed in the present work, the maximum absorbance was shown at 236nm for MET, 256nm for VOG and 268nm for PIO. The concentration range was 5-25, 0.2-1 and 2-10μg/mL with correlation coefficient 0.0998, 0.999 and 0.999 for MET, VOG and PIO respectively. The various parameters, such as linearity, system suitability, accuracy, precision, ruggedness, limit of detection and limit of quantification were studied as per ICH guidelines. Accuracy of the method was verified by performing recovery studies using simultaneous equation method and found to be 100.04-100.48% for MET, 98.70-99.70% for VOG and 98.67-100.27% for PIO indicates good accuracy of the method. Excellent mean recovery studies for precision, repeatability, ruggedness and sensitivity results showed that the method has been validated successfully, the results are also in accordance with the % RSD values obtained within specified limits. The proposed method was applied to the determination of MET, VOG and PIO, the mean % amount was found to be 100.21 (MET), 98.70 (VOG) & 101.28 (PIO) with % RSD values NMT 2.0% indicates the developed method was successfully applied for analysis of marketed formulation. The developed spectrophotometric method can be employed for routine analysis of MET, VOG and PIO in bulk and tablet formulation.

A New Analytical Method for Determination and Quantification of Residual Solvents in Relugolix Api Bulk Drug by GC-MS Method

A New Analytical Method for Determination and Quantification of Residual Solvents in Relugolix Api Bulk Drug by GC-MS Method

RP-HPLC Method Development and Validation for Determination of Abemaciclib in Bulk Drug Substance and Pharmaceutical Dosage Forms

A simple, economic, rapid and precise method for the quantification of Abemaciclib in bulk drug substance and pharmaceutical dosage forms was developed and validated using RP-HPLC. The chromatographic separation was achieved using Ascentis® C-18 HPLC column (250mm x 4.6mm i.d., particle size 5µ) with mobile phase containing 0.5% TFA: methanol: acetonitrile (35:45:20 v/v/v) with flow rate of 1.2mL/ min was used and effluents were monitored at 295nm. The retention time of Abemaciclib were found to be 3.72 min. The linearity was in the range of 6-42μg/mL. The limit of detection and limit of quantification were found to be 0.6 and 1.8 µg/mL, respectively. The % recoveries were found to be in the range of 99.65±0.77.
 Keywords: Abemaciclib, Estimation, Bulk drug substance, Pharmaceutical dosage forms

A stability indicating method development and validation of a rapid and sensitive RP-HPLC method for Nintedanib and its application in quantification of nanostructured lipid carriers

Background: Nintedanib (NTB) is a multiple tyrosine kinase inhibitor, been investigated for many disease conditions like idiopathic pulmonary fibrosis (IPF), systemic sclerosis interstitial lung disease (SSc-ILD) and non-small cell lung cancer (NSCLC). NTB is available as oral capsule formulation, but its ability to detect degradants formed through oxidative, photolytic and hydrolytic processes makes it difficult to quantify. In the current work, a novel reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated. Methods: The developed method is simple, precise, reproducible, stable and accurate. The inherent stability of NTB was evaluated using the proposed analytical method approach and force degradation studies were carried out. NTB was separated chromatographically on the Shimadzu C18 column as stationary phase (250 ×4.6 mm, 5 µm) using an isocratic elution method with 0.1% v/v triethyl amine (TEA) in HPLC grade water and acetonitrile (ACN) in the ratio 35:65% v/v. The mobile phase was pumped at a constant flow rate of 1.0 ml/min, and the eluent was detected at 390 nm wavelength. Results: NTB was eluted at 6.77±0.00 min of retention time (tR) with a correlation coefficient of 0.999, the developed method was linear in the concentration range of 0.5 µg/ml to 4.5 µg/ml. The recovery rate was found to be in the range of 99.391±0.468% for 1.5 µg/ml concentration. Six replicate standards were determined to have an % RSD of 0.04. Conclusion: The formulation excipients didn't interfere with the determination of NTB, demonstrating the specificity of the developed method. The proposed approach of the analytical method developed can be used to quantify the amount of NTB present in bulk drugs and pharmaceutical formulations.

Simultaneous Analysis of Ezetimibe and Rosuvastatin by Q absorption Ratio Method

A Novel UV spectrophotometric method has been developed for the simultaneous estimation of ezetimibe and rosuvastatin based on Q absorption ratio method. The wavelengths of 234.8nm (lsosbestic point) and 242nm (λmax of rosuvastatin) were chosen as analytical wavelengths. The linearity was established in concentration range 2-40µg/mL for ezetimibe and rosuvastatin with correlation coefficient greater than 0.990. Analytical method validation was performed by following ICH guidelines. The % assay for ezetimibe and rosuvastatin in tablet formulation complied with acceptance criteria. The developed method thus can be used as a powerful quality control tool for simultaneous analysis of the drugs in bulk and in formulation by UV spectroscopy.

A Novel Approach to AQbD-Assisted Green and Robust UPLC Method for the Determination of Selected Aminoquinoline Antimalarial Drugs: Assessment of Green Method

Greening analytical procedures have gained popularity in the area of pharmaceutical industries in order to safeguard the environment. In this study, an innovative methodology by integrating analytical quality-by-design (AQbD) along with Green Chemistry concepts with a systematic approach has been used to develop an environmentally-friendly and more robust ultra performance liquid chromatography (UPLC) method for the determination of three selected aminoquinoline antimalarial drugs namely amodiaquine hydrochloride (AMD), chloroquine phosphate (CHQ) and piperaquine phosphate (PPQ). An environmentally benign solvent ethanol has been chosen as an alternative to the commonly used acetonitrile and methanol, which are widely used. Based on the comprehensive risk analysis, the critical method parameters (CMP’s) that affect the critical method attributes (CMA’s) have been identified and the final method parameters were further optimized with the help of a full factorial design and the design of experiments (DOE), established the “design space”(DS) and identified the “method-operable-design-region (MODR) for the developed method. Achieved the separation with the use of an Acquity- UPLC BEH Shield RP-18 (100 mm × 2.1 mm), 1.7 μm column by using an isocratic elution of mobile phase containing 0.1% trifluoroacetic acid in water, ethanol in a mixture of 90:10% v/v and maintained a flow rate of 0.2 mL min-1 and the column oven temperature was 40 ºC and the UV detection wavelength of 225 nm was employed. A statistical tool Analysis of Variance (ANNOVA) has been used to assess the model’s statistical significance and found that the model’s p-values is < 0.00005 and its lack of fi is > 0.05 respectively, which demonstrates that the selected model is the most appropriate predictive tool for the analyzed responses R1 & R2 (i.e. peak resolutions R1 & R2). The proposed method’s linearity, accuracy & precision studies has been successfully validated in compliance with USP <1225> and ICH Q2 (R1) guidelines. Further assessed the proposed method’s greenness using various green evaluation tools such as: “complex green analytical procedure index”-cGAPI, “analytical greenness”-AGREE, “analytical method green score”-AMGS and found acceptable results. This novel AQbD-assisted eco-friendly analytical method for the quantification of AMD, CHQ & PPQ in bulk drugs (APIs) or finished dosage forms is simple, rapid, precise and accurate, robust and environmentally benign.

Mathematical Modeling of coupled tank interacting system for controlling water level using GWO and PSO optimization

In bulk drug production industries water level control at a precisepoint is a major dispute. Loss in production at the initial stageis observed until the water level reaches desired level. Pharmaceuticalindustries can however earn more profit if they could maintainprecise water level control at the initial stage of production. To synchronizethe water level precisely having best performance parameters,this work introduces Particle Swarm Optimization (PSO) and GreyWolf Optimization (GWO). By determining the mathematical model,the method for water proportion (level) control in the bridged tanksfor the MIMO system may be accomplished. The prior step for systemidentification is by observing the open-loop response of the system.This can be processed by analyzing the actual parameters of the coupledtank. State-space analysis of coupled tanks is explained in detailalong with its conversion into transfer function. In this paper, theinherent parameters required for the calculation are discussed. MATLABis used as the platform for observing the responses. Observationsfrom the PID controller articulate that, there is a need for a better controllerto enhance the performance. Performance analysis along withits discussion is conferred in this paper.

Development and Application of a Validated HPLC Method for the Determination of Alpelisib and its Process-Related Impurities in Pure Drug and Pharmaceutical Formulations

Impurity analysis plays a significant role in the manufacture of a safe pharmaceutical product that ensures the safety of consumers. Keeping this in consideration, the present study was intended to develop a simple and sensitive HPLC method for the resolution and quantification of 4 process-related impurities namely impurities 1, 2, 3 and 4 in alpelisib pure drug and formulations. The method consumes greener solvents as a mobile phase that resolves the analytes on ProntoSIL ODS-C18 (250×4.6 mm; 5 μ id) column at room temperature as stationary phase, ethanol and 0.1% aqueous acetic acid in 65:35 (V/V) at pH 4.5 as mobile phase at 0.8 mL/min flow rate, UV detection at 246 nm. The method can detect the analytes at retention times of 7.05, 4.52, 6.09, 2.88 and 8.14 min respectively for alpelisib, impurity 1, 2, 3 and 4. The analysis was completed with a run time of 15 min that consume less solvent and the same analysis time. The linearity of the proposed method was perceived in the range of 12.5 to 100 μg/mL for alpelisib and 0.0125 to 0.10 μg/mL for impurities. The method can effectively resolve the unknown stress degradation products generated during the stress exposure of alpelisib along with its known impurities in the study. The outcomes of other validation studies were likewise satisfactory and proven adequate for regular analysis of alpelisib and its process-related impurities in bulk drug and pharmaceutical tablet doses.

Validated Analytical Method for Multicomponent Analysis of Famotidine and Ofloxacin in Bulk drug and Tablet Formulation by using UV-Visible Spectrophotometer and RP-HPLC

A simple, sensitive, accurate, precise, and reproducible UV- spectrophotometric method and RP-HPLC methods were developed and validated for the estimation of Famotidine and Ofloxacin in bulk drug and pharmaceutical formulation. The Linearity regression was detected and shows a good linear relationship; in the concentration range of 10-50µg/mL (R2 >0.9908) for famotidine and 10-50µg/mL (r2>0.9913) for ofloxacin. The UV – spectrophotometric estimation was carried out by the first-order derivative spectrophotometric method and absorbance were recorded at 273 and 280nm. Beers range were found to be 5-50µg/mL, respectively for both drugs while, correlation coefficient r2 > 0.9988 and 0.9941 for famotidine and ofloxacin. The isoabsorptive point was found to be 274nm in HPLC optimized mobile phase composition, potassium dihydrogen orthophosphate: methanol (60:40). Chromatographic condition consisted of mobile phase potassium dihydrogen orthophosphate buffer pH 2.3, methanol (60:40v/v), run time 30 min, C-18 column (ODS Hypersil) and flow rate 0.8mL/minute. The retention time for famotidine and ofloxacin were found to be 2.44 min, 7.99 min. respectively, and detection at λmax 274nm for both drugs (overlain spectra). The UV methods and RP-HPLC showed good reproducibility and recovery with the percent relative standard deviation (RSD) less than 5%. As per ICH guidelines, the developed method was validated for linearity, accuracy, precision, Sandell's sensitivity, and repeatability proving its utility in the estimation of famotidine and ofloxacin in house tablet formulation.

An Ecofriendly Novel Spectrophotometric Estimation and Validation of Meloxicam in Bulk Drug and their Dosage Form by mixed Hydrotropic Solubilization Method

Solubility is a crucial factor during estimation of poorly soluble drugs. Literature survey reveals spectrophotometric estimation of poorly soluble drugs are mostly done by employing organic solvents. The drawbacks of organic solvents include higher cost, toxicity, pollution and error due to volatility. Hydrotropic solubilisation method involves increasing the solubility of a poorly soluble drug in water with the addition of hydrotropic agents. Most of NSAIDs like Meloxicam, Mefenamic acid, Aceclofenacetc are poorly soluble in water. Meloxicam was found to be soluble in mixed hydrotropic solution of 10% sodium benzoate and 10% sodium caprylate with maximum absorbance at 364 nm. The developed method was found to be linear in the range of 2-10 µg/ml with correlation coefficient (R2) of 0.9968. The LOD and LOQ of proposed method was found to be 0.2634 µg/ml and 0.7983 µg/ml respectively. A novel, simple, safe, sensitive and cost-effective spectrophotometric estimation method was developed for estimation of Meloxicam using 10% sodium benzoate and 10% sodium caprylate as hydrotropic agent. This solubilization method can be employed to preclude the use of organic solvents for the estimation of poorly soluble drugs.

Simultaneous Estimation of Adapalene from Marketed Gel Formulation along with the Preservative Phenoxyethanol by UV- Visible Spectroscopy

A simple, rapid and eco-friendly UV spectroscopic method was developed for the estimation of Adapalene along with Phenoxyethanol for laboratory purpose. Bulk drug and marketed formulation both are analyzed and validated by this method. Tetrahydrofuran was selected for the solubility of Adapalene and Phenoxyethanol as per solubility profile. Wavelength selected for Adapalene and Phenoxyethanol was 325nm and 269nm respectively. In the proposed method, adapalene and phenoxyethanol follows linearity in the concentration range 1-5µg/mL and 2.5-12.5µg/mL with a correlation coefficient 0.999 and 0.998 respectively. Proposed method was statistically validated as per ICH guidelines and by recovery studies. The standard deviation was found to be less than 2, which showed excellent precision and accuracy.

Analytical RP-HPLC method development and validation for simultaneous estimation of Emtricitabine, Tenofovir and Bictegravir

The Emtricitabine, Bictegravir and Tenofovir are used to treat Cystic fibrosis treatment. For estimation of this drug in bulk and pharmaceutical dosage form the standard, simple, accurate RP-HPLC method was devoloped, to run the sample column used was Kromasil C18 150×4.6mm,5µ and mobile phase of 0.1%OPA and acetonitrile of 55:45 v/v at a flow rate of 1ml/min, 30°C temperature was maintained, 272.0 nm wavelength was used. The retention times for tenofovir, bictegravir, and emtricitabine were 2.140,2.432, and 2.992 minutes, respectively. Emtricitabine, Bictegravir, and Tenofovir were found to have 1.1, 1.0, and 0.9 percent RSD of method precision respectively. Emtricitabine, Bictegravir, and Tenofovir all recovered 100.24 percent, 100.19 percent, and 100.06 percent of their doses, respectively and LOQ values are 0.93 ppm, 0.34 ppm and 0.23ppm respectively, and LOQ values are 2.80ppm, 1.04, 0.70ppm, respectively, for Emtricitabine, Bictegravir, and Tenofovir.

Development and validation of a stability-indicating assay method for determination of metronidazole benzoate in bulk: Spectroscopic approach

A new, simple, rapid, accurate, sensitive and cost effective spectrophotometric stability indicating assay method was developed for the quantification of metronidazole benzoate in bulk and validated according to ICH guidelines using different parameters. In the present study an attempted has been made to develop an effective method which will surpass the disadvantages associate with other reported methods like tedious in use, less sensitive and costly etc. The assay method was based on the forced degradation study of metronidazole benzoate under different ICH recommended stress conditions like hydrolytic, oxidation, thermal, and photolysis. Drug shown maximum absorption at 322nm and a regression coefficient value (R2) of 0.999 indicates linearity followed within the concentration range of 5µg/ml to 50µg/ml. During forced degradation study, metronidazole was significantly degraded in alkaline conditions whereas mild degradation occurs in acidic, neutral and oxidative stress. The drug was stable to dry heat and photolytic degradation conditions. Statistical validation result of the developed method indicates that it was a simple, precise, reproducible, selective, specific and accurate method for analysis of Metronidazole and could be successfully adopted to estimate the drug in bulk and formulations.