Commercial Dosage Forms Research Articles

Utilizing erythrosine B absorption spectrum shifts for quantitative determination of octreotide and bromocriptine in their pure forms and pharmaceutical formulations. Evaluation of the method greenness

In the present study, two drugs for treating acromegaly are investigated which are either synthetic growth hormone inhibiting hormone (GHIH) or dopamine receptor agonist. Octreotide (OCT) and bromocriptine (BCT) were quantified with a quick, simple, and sensitive spectrophotometric approach in their authentic forms and commercial dosage forms. This approach was based upon formation of ion pair complex between erythrosine B and investigated drugs in an aqueous buffered solution. For OCT determination the higher sensitivity was obtained using ΔA at 525 nm. On the other hand, BCT was estimated using the absorbance at 556 nm. Under optimal conditions for the reaction, construction of calibration curves were performed within concentration range of 0.4–4 µg ml−1 for OCT and 1–9 µg ml−1 for BCT with with low detection limits (0.094 and 0.235 µg ml−1) and low quantitation limits (0.29 and 0.71 µg ml−1) for OCT and BCT respectively. The developed approach was assessed for linearity, accuracy, precision, limits of detection, and limits of quantitation in compliance with ICH validation recommendations. The suggested approaches demonstrated good linearity, as evidenced by determination coefficients (r2) of 0.999 with a slope 0.14 for OCT and 0.9989 with a slope 0.06 for BCT. Additionally, the environmental friendliness of the investigated method was assessed with some of the recent green analytical chemistry metrics.

ANALYTICAL TECHNIQUES FOR DETERMINATION OF MIRABEGRON FROM BULK, PHARMACEUTICAL FORMULATION, AND BIOLOGICAL MATRICES: A CRITICAL REVIEW

Mirabegron is a beta-3 adrenergic receptor agonist and is specified for the treatment of overactive Bladder. This review covers analytical methods aimed at the identification and quantification of mirabegron in bulk, commercial dosage forms, and Biological fluids. Using various techniques such as UV-spectroscopy, spectro-fluorimetry, planer chromatography, High Performance-Thin Layer Chromatography (HPTLC), HPLC, High-Performance Liquid Chromatography-MS/MS (HPLC-MS/MS), Ultra-Pressure Liquid Chromatography-MS/MS (UPLC-MS/MS), and capillary electrophoresis. HPLC is the most used analytical technique for the identification and quantification of mirabegron in bulk and commercial dosage forms.

Development of a novel UPLC approach to co-prediction of four active compounds in a multi-component pharmaceutical preparation

In this work, a new ultra-performance liquid chromatography method based on photodiode array detection (UPLC-PDA) was first developed for the quantitative analysis of the quaternary mixture of ascorbic acid (AA), paracetamol (PAR), caffeine (CAF) and chlorpheniramine maleate (CPA) in a commercial dosage form. The developed UPLC-PDA method offered a new possibility for the co-determination of four active ingredients in a drug combination with short run time and simple sample preparation. The successful chromatographic separation of the four drugs was performed using a Waters Acquity UPLC BEH C18 column (1.7 µm 2.1 × 100 mm) (Mildford, USA) and a mobile phase consisting of water (12 %), acetonitrile (13 %) and 0.1 M H3PO4 (75 %) at a flow rate of 0.25 mL/min. The validation of the proposed UPLC-PDA approach was verified by analyzing synthetic mixtures, inter- and intra-day experiments, and commercial powder samples and provided satisfactory results.

First derivative synchronous spectrofluorimetric method for the simultaneous determination of tramadol and celecoxib in their dosage forms and human plasma.

One of the most common features of many different clinical conditions is pain; hence, there is a crucial need for eliminating or reducing it to a tolerable level to retrieve physical, psychological and social functioning. A first derivative synchronous spectrofluorimetry technique is proposed for the simultaneous determination of celecoxib and tramadol HCl, a recent coformulation authorized for treating acute pain in adults. The method includes using synchronous spectrofluorimetry at ∆λ = 80 nm where tramadol HCl was determined using first derivative technique at λ = 230.2nm, while celecoxib was determined at λ = 288.24 nm. The proposed method was successfully applied to their co-formulated dosage forms in addition to spiked human plasma and validated in agreement with the guidelines of the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The linear ranges were found to be 0.50-5.0 and 0.15-0.50, the limits of detection to be 0.088 and 0.011 and the limits of quantification to be 0.266 and 0.032 μg/ml for celecoxib and tramadol, respectively. Statistical analysis revealed no significant difference when compared with previously reported methods as evidenced by the values of the variance ratio F-test and Student t-test. The proposed method was successfully applied to commercial dosage forms and spiked human samples. Moreover, the greenness of the proposed method was investigated based on the analytical eco-scale approach, with the results showing an excellent green scale with a score of 95.

A Validated RP-HPLC Method for Simultaneous Quantification of Abacavir and Zidovudine and their Impurities in Combined Dosage Forms

Develop a simple, accurate, and precise method for simultaneous analysis of Abacavir and Zidovudine, along with their related impurities, in combined pharmaceutical dosage forms. A reverse- phase high-performance liquid chromatography (RP-HPLC) method was developed using an LC-20 AT C18 column and a Water: Methanol (80:20) mobile phase. Detection was carried out at 240 nm. The method successfully separated Abacavir, Zidovudine, and their respective impurities with distinct retention times. Validation demonstrated good linearity, accuracy, and precision for both drugs and their impurities. Limits of detection (LOD) and quantification (LOQ) were determined and found to be suitable for analyzing impurities in commercial dosage forms. The developed RP-HPLC method offers a simple, accurate, and reliable tool for simultaneous quantification of Abacavir, Zidovudine, and their impurities in combined dosage forms, thereby contributing to quality control and ensuring drug safety. Keywords Abacavir, Zidovudine, Related Substance RP-HPLC Method, ICH Q2 (R1) guidelines

Development and Validation of Dissolution Test Method for Herbal Medicine Containing Ginsenosides

Background and objective: This study aimed to develop a dissolution test method for quality control of commercial 40% ethanol extract of ginseng-containing dosage forms.Methods: Through preliminary dissolution testing of the commercial dosage forms, suitable parameters for HPLC (high performance liquid chromatography) analysis were determined, including an injection volume of 50 μL and a dissolution time of 1 hour. Additionally, the stability testing of the solution enabled the selection of an appropriate dissolution medium, pH 4.0 buffer solution. Method validation was carried out using reference standard of eight ginsenosides (Rg1, Re, Rf, Rg2, Rb1, RC, Rb2, Rd), indicative components of ginseng, under the selected testing conditions. The evaluation of method validation encompassed specificity, accuracy, precision, and linearity as assessment criteria.Results: The accuracy assessment revealed that the average recovery rates within a 95% confidence interval were appropriate for all ginsenosides, ranging from 98.25% to 101.17%. The precision evaluation, conducted at an intermediate concentration of 8 μg/mL (n = 6), demonstrated relative standard deviations of 0.25% to 1.08%, which met the criterion of being below 2%. The linearity assessment showed that the coefficient of determination (R²) values for all ginsenosides exceeded 0.999, indicating excellent linearity. The quantification limits ranged from 0.32 to 1.09 μg/mL, confirming their suitability for dissolution assessment of the respective formulation. Employing the selected dissolution test method, the dissolution profiles of most ginsenosides in the commercially available ginseng-containing dosage forms reached their maximum values within 60 minutes. No significant differences were observed in results beyond 120 minutes, confirming that a dissolution time of 60 minutes is appropriate for this dosage form.Conclusion: The established method holds promise as a valuable tool for quality control of pharmaceuticals containing ginseng, including those previously unassessed, contributing to future applications in the pharmaceutical industry.

RP-HPLC Method for the Simultaneous Determination of Sofosbuvir and Daclatasvir in Pure and Pharmaceutical Dosage Forms

Daclatasvir and sofosbuvir in pure and medicinal dosage forms can be determined quickly and easily using a reversed-phase high-performance liquid chromatography (RP-HPLC) technique. An accurate, reproducible method was developed and validated. The mobile phase contained a mixture of 90% methanol:10% water (0.05% OPA). UV estimation was done with a flow rate of 0.7 mL/min and wavelength of 275 nm. The temperature was 30°C. Sofosbuvir stays in the body for 3.361 minutes and daclatasvir for 5.745 minutes. A quantitative study of commercial dosage forms went well with this method, which was made and tested. Sofosbuvir and daclatasvir each had a %RSD of 0.43 and 0.28, respectively. Recoveries were 97.85 and 98.52% for sofosbuvir and daclatasvir, respectively. Three methods were checked for precision, accuracy, linearity, selectivity, specificity, limit of detection (LoD), limit of quantitation (LoQ), robustness, and ruggedness according to rules of the International Council for Harmonisation (ICH).

Thermosensitive Polyurethane-Based Hydrogels as Potential Vehicles for Meloxicam Delivery.

Meloxicam (MX) is a nonsteroidal anti-inflammatory drug (NSAID) used mainly to reduce pain, inflammation, and fever. In the present study, thermosensitive polyurethane (PU)-based hydrogels with various excipients (PEG, PVP, HPC, and essential oil) were prepared and loaded with MX. Rheological investigations were carried out on the PU-based formulations in various shear regimes, and their viscoelastic characteristics were determined. The average size of the PU micelles was 35.8 nm at 37 °C and slightly increased at 37 nm in the presence of MX. The zeta potential values of the hydrogels were between -10 mV and -11.5 mV. At pH = 6 and temperature of 37 °C, the formulated PU-based hydrogels loaded with MX could deliver significant amounts of the active substance, between 60% and 80% over 24-48 h and more than 90% within 2 weeks. It was found that anomalous transport phenomena dominated MX's release mechanism from the PU-based networks. The results are encouraging for further studies aiming to design alternative carriers to commercial dosage forms of nonsteroidal anti-inflammatory drugs.

Development and Comparative Evaluation of Two Different Label-Free and Sensitive Fluorescence Platforms for Analysis of Olaparib: A Recently FDA-Approved Drug for the Treatment of Ovarian and Breast Cancer.

Olaparib (OLA) is a PARP inhibitor drug which has been recently approved by the Food and Drug Administration (FDA) for the treatment of ovarian and breast cancer. A convenient analytical tool for the quantitation of OLA in its dosage form and plasma samples was urgently needed. This study describes, for the first time, the development of two different label-free and sensitive fluorescence-based platforms for the pharmaceutical and bioanalysis of OLA. These platforms were microwell-assisted with a fluorescence microplate reader (MW-FLR) and high-performance liquid chromatography with fluorescence detection (HPLC-FD). Both MW-FLR and HPLC-FD employed the native fluorescence of OLA as an analytical signal. The MW-FLR involved measuring the fluorescence signals in 96-well white-opaque plates. The HPLC-FD involved chromatographic separation of OLA and duvelisib (DUV), as an internal standard on a Nucleosil-CN HPLC column (250 mm length × 4.6 mm i.d., 5 µm particle diameter) with a mobile phase composed of acetonitrile: water (25:75, v/v) pumped at a flow rate of 1.7 mL/min. Elution of OLA and DUV was detected using a fluorescence detector. The optimal conditions of both MW-FLR and HPLC-FD were established, and they were validated according to the guidelines of the International Council for Harmonization for the validation of analytical procedures. The linear ranges of MW-FLR and HPLC-FD were 25-1000 and 5-200 ng/mL, respectively, with limits of detection of 15 and 1.7 ng/mL, respectively. The accuracy and precision of both platforms were confirmed as the recovery values were ≥98.2% and the relative standard deviations (RSD) were ≤2.89%. Both methodologies were satisfactorily applied to the quantitation of OLA in its commercial dosage form (Lynparza® tablets) and plasma samples with high accuracy and precision. The greenness of both MW-FLR and HPLC-FD was assessed using two different multiple parameter-based metric tools, and the results proved their greenness and adherence to the requirements of green analytical approaches. Both platforms have simple procedures and acceptable levels of analytical throughput. In conclusion, the proposed MW-FLR and HPLC-FD are valuable tools for routine use in quality control and clinical laboratories for the quantitation of OLA for the purposes of pharmaceutical quality control, pharmacokinetic studies, and bioequivalence testing.

Review Article on Inprocess Problems and Evaluation Tests of Tablets Manufacturing

Tablets are the traditional over all medicinal dosage forms for solid dosages. A tablet is a solid pharmaceutical dosage form that is typically manufactured by compressing or moldings the medicinal component with appropriate diluents. They are easier to create than any other dosage form, but during manufacturing, a number of issues may occur that force the batch to be discarded. Post compression studies are also crucial before the dosage forms are put on the market. Modern standards and concepts that emphasize bioavailability, bioequivalence, and validation, among other things, have an impact on formulation design and production. In this article, we discussed the issues (Picking, Sticking, Mottling, etc.) that will arise during the production of tablets, their solutions, as well as the pre- and post- Compression qualities (such as hardness, thickness, and weight variation) and the upper limitations of their use in commercial dosage forms.

New analytical LC–MS/MS method for fluconazole and ivermectin estimation in combined pharmaceutical dosage form: development and validation

BackgroundFluconazole, an antifungal drug, prevents fungi growth by inhibiting the formation of a protective covering. Ivermectin has several biological activities, such as antibacterial, antiviral, and anti-cancer characteristics, and offers various therapeutic outcomes. There are several commercial products containing these two drugs. Therefore, developing a method that can allow the simultaneous estimation of Fluconazole and ivermectin is inevitable to monitor them in commercial dosage forms. The hyphenated methodology that combines spectroscopic and chromatographic techniques is gaining high interest in the pharmaceutical industry. Consequently, the objective of present research work was to investigate robust and sensitive LC–MS/MS avenue for simultaneous determination of Fluconazole and ivermectin in pure material and combined dosage form.ResultsThe simultaneous quantification of Fluconazole and ivermectin in tablet dosage form has been developed and validated using a straightforward, sensitive, practical, and repeatable LC–MS/MS approach. The separation was performed using a C18 (150 × 4.6 mm) column, injection volume of 10 µL, and elution with acetonitrile: formic acid at a ratio of 70:30, with the column temperature at 30 °C, and a flow rate of 4.0 mL/min. The retention times of Ivermectin and Fluconazole were 1.10 min and 1.05 min, respectively. The calibration curves for Fluconazole and ivermectin demonstrated significant linearities indicated by the correlation coefficients (r2 = 0.999 and r2 = 0.997) and precision (% R.S.D. of 1.58 and 1.13). The linear correlation between peak area and concentration allowed high percentage recoveries of 98.5%–99.4% and 97.8%–99.3% for Fluconazole and Ivermectin, respectively. The L.O.D.s for Fluconazole and ivermectin were found to be 0.0034 and 0.074 g/mL, respectively. The L.O.Q.s for Fluconazole and ivermectin were 0.010 and 0.225 g/mL, respectively.ConclusionAll the analytical parameters were identified and found to be within the acceptable range set forth by the ICH guidelines, demonstrating the devised method's acceptability in the simultaneous detection and estimation of Fluconazole and ivermectin in the commercial dosage forms.

Stability Indicating RP-HPLC Method Development and Validation for the determination of Pretomanid an anti-bacterial drug

A new simple, rapid, accurate and stability indicating RP-HPLC method have been developed and validated for estimation of Pretomanid is an anti-bacterial agent in pharmaceutical dosage form. The RP-HPLC analysis was performed by using Xtimate C18 column (250mm × 4.6mm; 5µm) with Methanol: Acetonitrile: Ammonium phosphate buffer in the ratio of 55:40:05 (v/v/v) as mobile phase at a flow rate of 1.0mL/min and detected at 262nm wavelength. The calibration curve was linear over the concentration range from 10 to 40µg/mL and correlation coefficient was found to be 0.99. LOD and LOQ were estimated as 0.30µg/mL and 5.0µg/mL respectively. The % recovery was achieved from 98.67% to 99.96%. The method was applied for estimation in its pharmaceutical dosage form and assay result was 98.9% label claim. Proposed method showed excellent linearity, accuracy, precision, specificity, robustness, LOD, LOQ, and system suitability results within the acceptance criteria as per ICH guidelines. The Pretomanid drug was subjected to stress condition of Hydrolysis, Oxidation, Photolysis and Thermal degradation, Forced degradation study was carried out and the degradation products were well resolved from the pure Pretomanid drug. The proposed method was successfully applied for the estimation of Pretomanid drugs in commercial dosage form.

Colon Target Drug Delivery System Review

For the local treatment of a number of bowel disorders such as ulcerative colitis, Crohn's disease, amoebiasis and sand, colonic cancer, the local treatment of colonic pathologies, and the systemic distribution of protein and peptide medicines, targeted drug delivery into the colon is extremely desirable. A medication must be properly formulated for colon-focused drug delivery. To ensure sudden or controlled release in the proximal colon, the substance must first be shielded from degradation, release, and absorption in the upper GI tract. The advantages and disadvantages, cutting-edge methods for colon-targeted drug delivery, clinical evaluation methods, and some details about commercial dosage forms are the main topics of this paper

Sulfur and nitrogen co-doped carbon quantum dots as fluorescent probes for the determination of some pharmaceutically-important nitro compounds

In this study, highly fluorescent sulfur and nitrogen co-doped carbon quantum dots (SN-CQDs) were synthesized by a simple one-pot hydrothermal method using thiosemicarbazide and citric acid as starting materials. Various spectroscopic and microscopic techniques were applied to characterize the prepared SN-CQDs. The synthesized SN-CQDs’ maximum fluorescence emission was obtained at 430 nm after excitation at 360 nm. Rifampicin (RFP), tinidazole (TNZ), ornidazole (ONZ), and metronidazole (MNZ) all quantitatively and selectively quenched the SN-CQDs’ native fluorescence, which was the base-for their-spectrofluorimetric estimation without the need for any tedious pre-treatment steps or high-cost instrumentation. SN-CQDs demonstrated a “turn-off” fluorescence response to RFP, TNZ, ONZ, and MNZ over the ranges of 1.0–30.0, 10.0–200.0, 6.0–200.0, and 5.0–100.0 μM with detection limits of 0.31, 1.76, 0.57, and 0.75 μM and quantitation limits of 0.93, 5.32, 1.74, and 2.28 μM respectively. The suggested method was successfully used to determine the investigated drugs in their commercial dosage forms. The method was further extended to their determination in spiked human plasma samples, with satisfactory mean % recoveries (99.44–100.29) and low % RSD values (< 4.52). The mechanism of fluorescence quenching was studied and discussed. The suggested method was validated in accordance with ICH recommendations.

A Validated, Stability-Indicating, Eco-Friendly HPTLC Method for the Determination of Cinnarizine

The eco-friendly high-performance thin-layer chromatographic (HPTLC) approaches for measuring cinnarizine (CIN) are scant in reported databases. As a result, the current work has developed and validated an eco-friendly HPTLC technique for assessing CIN in commercial formulations. The proposed approach was based the use of ethyl alcohol-water (90:10 v/v) as the eco-friendly mobile phase. A wavelength of 197 nm was used to detect CIN. The greenness score of the current approach was measured using the Analytical GREENness (AGREE) approach. The current approach was linear for CIN measurement in 50–800 ng band−1 range. The current approach for CIN measurement was validated successfully using ICH guidelines and was found to be linear, accurate (% recovery = 99.07–101.29%), precise (% CV = 0.80–0.95%), robust, sensitive (LOD = 16.81 ng band−1 and LOQ = 50.43 ng band−1), specific, selective, stability-indicating, and eco-friendly. The AGREE score for the current approach was calculated to be 0.80, showing an excellent greenness characteristic of the present approach. Under forced degradation conditions, the current approach was successful in separating the CIN degradation product, demonstrating the stability-indicating qualities/selectivity of the present approach. The % assay of CIN in commercial tablet brands A and B was found to be 98.64 and 101.22%, respectively, suggesting the reliability of the present approach in the pharmaceutical analysis of CIN in commercial dosage forms. The obtained findings indicated that CIN in commercial formulations could be routinely determined using the current approach.

HPLC-Fluorescence Detection Method for Concurrent Estimation of Domperidone and Naproxen. Validation and Eco-Friendliness Appraisal Studies

This work demonstrates a simple and reliable HPLC method with fluorimetric detection for simultaneous estimation of domperidone (DOM) and naproxen (NAP). Successful chromatographic separation was accomplished using Inertsil ODS C18 column (5 μm, 4.6 × 150 mm) with gradient elution of the mobile phase consisting of 0.01 M phosphate buffer (pH 5.5) solution and acetonitrile. The gradient elution started with 25% acetonitrile increased linearly to 65% in 5 min, then kept at this percentage till the end of the run. The mobile phase was pumped at a flow rate of 1.0 mL/min. The excitation wavelength at 284 nm was found suitable for both DOM and NAP since it corresponds to a maximum for the minor component DOM and measurable excitation for NAP, while using 316 and 355 nm as emission wavelengths for DOM and NAP, respectively. Peaks eluted with excellent resolution at retention times 4.4 and 6.3 min for DOM and NAP, respectively. Performance of the proposed method was tested according to ICH guidelines in regard to linearity, ranges, precision, accuracy, robustness, detection and quantitation limits. Calibration curves were linear in the ranges of 0.8–3.6 and 1.0–2.5 µg/mL for DOM and NAP respectively with correlation coefficients not less than 0.9996. The validated method was successfully applied to the analysis of DOM and NAP in their laboratory prepared tablets resembling the commercial dosage form, and assay results were favorably compared with a published reference HPLC method. The method’s greenness was assessed using the Analytical Eco-Scale and the novel Analytical Greenness metric (AGREE).

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF TINIDAZOLE AND FLUCONAZOLE AND ITS APPLICABILITY IN MARKETED DOSAGE FORM

Objective: The current method is focused on the development and validation of a simple, rapid, precise and robust stability indicating High Performance Thin Layer Chromatography for the simultaneous estimation of anti-infective drugs Tinidazole and Fluconazole in bulk and its pharmaceutical dosage form. The method was tailored to analyse the drugs in their commercial dosage form (tablets) with no interference from ingredients. Methods: Chromatographic separation was performed over precoated TLC plates (60 F254, 20 cm × 10 cm, 250 μm thickness, Merck) via a linear ascending technique using toluene: acetonitrile as the mobile phase in the ratio 6:4 v/v. Detection and quantification was achieved at the isobestic point of the two drugs, which was observed at 263 nm through Spectro-densitometric analysis. Analytical performance of the proposed HPTLC method was validated according to the ICH guidelines with respect to the linearity, accuracy, precision, detection and quantitation limits, robustness and specificity. Results: Tinidazole and Fluconazole were well separated and identified with an Rf value of about 0.46±0.03 and 0.75±0.05, respectively. The calibration curves were linear over a concentration range of 800-1200ng/spot for Tinidazole and 60-90ng/spot for Fluconazole with correlation coefficients (r2) more than 0.998. The above-developed method was validated as per ICH guidelines Q2(R1) and was found to be precise, sensitive, accurate and robust. Conclusion: The validated stability indicating HPTLC method was found to be simple, precise, accurate and sensitive for the concurrent quantification of Tinidazole and Fluconazole in pharmaceutical dosage form and can be released into quality control for regular analysis.

Multivariate calibration technique for spectrophotometric quantification of ondansetron in bulk drug and pharmaceutical formulations

The aim of the present work to develop an accurate, simple, sensitive, and validated Ultra violet (UV) spectrophotometric procedure using multilinear regression method for the analysis of Ondansetron in its bulk and commercial dosage form. The multivariate calibration approach was based on equations constructed using linear regression analysis using the correlation between absorbance and concentration at selected five different wavelengths. Ondansetron had a maximum wavelength of 246 nm. The findings were statistically analysed. A linear plot in the concentration range of 5-15 µg/mL, with a regression co-efficient of 0.999 was obtained. The % RSD for intra-day and Inter day precision were 0.0409 and 0.0228, respectively. The assay was determined and found to be 98.38 % – 101.10 % w/w.

Atropine-Phosphotungestate Polymeric-Based Metal Oxide Nanoparticles for Potentiometric Detection in Pharmaceutical Dosage Forms.

The new research presents highly conductive polymeric membranes with a large surface area to volume ratio of metal oxide nanoparticles that were used to determine atropine sulfate (AT) in commercial dosage forms. In sensing and biosensing applications, the nanomaterials zinc oxide (ZnONPs) and magnesium oxide (MgONPs) were employed as boosting potential electroactive materials. The electroactive atropine phosphotungstate (AT-PT) was created by combining atropine sulfate and phosphotungstic acid (PTA) and mixing it with polymeric polyvinyl chloride (PVC) with the plasticizer o-nitrophenyl octyl ether (o-NPOE). The modified sensors AT-PT-ZnONPs or AT-PT-MgONPs showed excellent selectivity and sensitivity for the measurements of atropine with a linear concentration range of 6.0 × 10−8 − 1.0 × 10−3 and 8.0 × 10−8 − 1.0 × 10−3 mol L−1 with regression equations of E(mV) = (56 ± 0.5) log [AT] − 294 and E(mV) = (54 ± 0.5) log [AT] − 422 for AT-PT-NPs or AT-PT-MgONPs sensors, respectively. The AT-PT coated wire sensor, on the other hand, showed a Nernstian response at 4.0 × 10−6 − 1.0 × 10−3 mol L−1 and a regression equation E(mV) = (52.1 ± 0.2) log [AT] + 198. The methodology-recommended guidelines were used to validate the suggested modified potentiometric systems against various criteria.

Development and Validation of Quality by Design based RP-HPLC Method for determination of Tenofovir Alafenamide Fumarate from Bulk drug and Pharmaceutical dosage form and its application to Forced Degradation Studies

The present research work entails the development and validation of a simple, robust and sensitive stability indicating reverse phase high performance liquid chromatographic method using Quality by Design methodology for estimation of Tenofovir alafenamide fumarate in bulk drug and its marketed dosage form. Chromatographic separation was performed in isocratic mode using Inertsil C18 column, mobile phase composed of Acetonitrile: ammonium formate buffer pH 5(40: 60) at a flow rate of 1mL/min with Photo Diode Array (PDA) detection at 261nm. A Box-Behnken statistical design with 3 factors and 3 levels was selected for the optimization study. Interaction effects of Critical Quality Parameters (Buffer pH, Organic Phase-% acetonitrile, flow rate) were evaluated for critical quality attributes (Retention time, NTP and symmetry factor). The optimized method was validated according to the current International Conference Harmonization (ICH) Q2 R1 guidelines. The method was found to be linear, covering the range from 1.5 μg/mL – 4.5 μg/mL with correlation coefficient r2 of 0.9996 and precision was found to be less than 2%. Limit of Detection and Limit of Quantification was found to be 1µg/mL and 1.2µg/mL respectively. Accuracy was between 99% and 102%. Forced degradation study was conducted under degradation conditions like light, oxidation, dry heat, acidic, basic, hydrolysis in order to establish the intrinsic stability of molecule. The method was successfully applied for the determination of the drug in commercial dosage form. This holistic stability indicating chromatographic method focused on QbD approach ensured reproducibility and was found to be useful for routine analysis of Tenofovir alafenamide fumarate.