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Background: The concurrent measurement of emtricitabine, tenofovir, and rilpivirine was achieved using UPLC, employing Analytical Quality by Design (AQbD) principles, which encompass response surface methodology (RSM) and Box–Behnken design (BBD). This approach offers a systematic and efficient method for improving analytical procedures and ensuring reliable results. Results: Analyte separation was accomplished using an Endoversil C 18 (2.1 × 50 mm, 1.7 µm) column as the stationary phase. The mobile phase consisted of a mixture of 80% orthophosphoric acid (0.1%) and 20% acetonitrile, with a flow rate of 0.4 ml/min and a column temperature of 30 °C. A photodiode array detector was used for detection at 270 nm. The peak area response-concentration curve exhibited linearity across ranges of 50–250 µg/ml (emtricitabine), 100–500 µg/ml (tenofovir), and 10–50 µg/ml (rilpivirine). Quantitation limits were determined to be 0.099 µg/ml (emtricitabine), 0.165 µg/ml (tenofovir), and 0.066 µg/ml (rilpivirine). The method was successfully validated for the simultaneous determination of emtricitabine, tenofovir, and rilpivirine in combined tablet dosage form. Percentage recoveries were 99.89%, 99.52%, and 100.20%, with relative standard deviations of 0.415%, 0.268%, and 0.559% for emtricitabine, tenofovir, and rilpivirine, respectively. Conclusion: The performance of the proposed method was evaluated against reported RP-UPLC methods and found to be rapid and cost-effective. The developed and validated stability indicating RP-UPLC method proved suitable for quality control and drug analysis. [ABSTRACT FROM AUTHOR]

The present research aims to establish new stability indicating RP-UPLC method for concurrently estimating Pregabalin and Etoricoxib in blended powder and their combined tablet formulation. The effective separation of Pregabalin and Etoricoxib achieved with HSS column C18 (150 × 2.1 mm, 1.8 µm), 0.1% orthophosphoric acid: acetonitrile in 65:35 v/v) at a flow rate of 0.3 mL/min, and isocratic elution at 228 nm. The elution of PRB and ETB was noticed at 1.56 and 2.01 min, with good resolution and system suitability with the developed approach. PRB and ETB have shown linear responses from 18.75 to 112.5 µg/mL and 15 to 90 µg/mL, respectively. The range of the % RSD for intraday and inter-day precision was 0.33 to 0.81. The LOD and LOQ of Pregabalin and Etoricoxib were computed to be 0.07 µg/mL, 0.21 µg/mL, and 0.01 µg/mL, 0.04 µg/mL, respectively, by standard deviation method. The validation method was carried out using ICH standards. The stability- indicating the feature of the method was confirmed by the forced degradation studies where degradants generated by stress testing were clearly distinguished from the peaks of analytes. The shorter elution period and superior sensitivity of both analytes with this method are appropriate for regular analysis of Pregabalin and Etoricoxib.Article Highlights: A new RP-UPLC method for analysis of Pregabalin and Etoricoxib in powder and tablet form. Simple mobile phase and economical column for separation of Pregabalin and Etoricoxib. Shorter retention time with isocratic elution and effective resolution. Greater sensitivity regarding LOD and LOQ. Stability indicating method through the forced degradation studies. [ABSTRACT FROM AUTHOR]

Abstract RP-HPLC technique was developed and optimized for simultaneous identification and estimation of nirmatrelvir (NIR) and ritonavir (RIT) in their new copackaged tablet. Stability of nirmatrelvir (NIR) was studied after exposure to different five stress conditions; alkali, acid, heat, photo and oxidation degradation. The chromatographic separation was achieved using VDSpher PUR 100 ODS (4.6-mm x 15-mm), 3.5 μm column and mixture of 0.03 M potassium di-hydrogen phosphate buffer pH 4 and acetonitrile (45:55, v/v) as mobile phase. The column temperature was set at 40 °C, flow rate at 1mL/min and UV detection at 215 nm. The NIR and RIT retention times were 3.94 ± 0.08 min and 9.08 ± 0.1 min, respectively. Linear relationship was established in range of (1.5–105 µg/mL) for NIR and (1–70 µg/mL) for RIT with good reproducibility. The found mean percentage recoveries of nirmatrelvir (NIR) and ritonavir (RIT) were 100.03% and 99.85%, respectively. The developed method shows very good sensitivity as the LOQ and LOD were found to be 3.001 & 0.990 µg/mL, respectively for NIR and 2.765 & 0.912 µg/mL, respectively for RIT. The developed approach was validated concerning to ICH guidelines and applied successfully for the simultaneous estimation of NIR and RIT in their new copackaged dosage from. The results of assay using the proposed approach were compared statistically to the results found by applying the published one with good agreement.

Abstract The present research aims to establish new stability indicating RP-UPLC method for concurrently estimating Pregabalin and Etoricoxib in blended powder and their combined tablet formulation. The effective separation of Pregabalin and Etoricoxib achieved with HSS column C18 (150 × 2.1 mm, 1.8 µm), 0.1% orthophosphoric acid: acetonitrile in 65:35 v/v) at a flow rate of 0.3 mL/min, and isocratic elution at 228 nm. The elution of PRB and ETB was noticed at 1.56 and 2.01 min, with good resolution and system suitability with the developed approach. PRB and ETB have shown linear responses from 18.75 to 112.5 µg/mL and 15 to 90 µg/mL, respectively. The range of the % RSD for intraday and inter-day precision was 0.33 to 0.81. The LOD and LOQ of Pregabalin and Etoricoxib were computed to be 0.07 µg/mL, 0.21 µg/mL, and 0.01 µg/mL, 0.04 µg/mL, respectively, by standard deviation method. The validation method was carried out using ICH standards. The stability- indicating the feature of the method was confirmed by the forced degradation studies where degradants generated by stress testing were clearly distinguished from the peaks of analytes. The shorter elution period and superior sensitivity of both analytes with this method are appropriate for regular analysis of Pregabalin and Etoricoxib. Graphical Abstract

Tavaborole, a topical antifungal agent containing Boron is used for the treatment of onychomycosis, an infection of the nail and nail bed caused by Trichophyton rubrum or Trichophyton mentagrophytes infection. Tavaborole is chemically known as 5 - Fluoro -1,3 - dihydro -2,1-benzoxaborol -1-ol. It acts by inhibiting Leucyl-tRNA synthetase an essential fungal enzyme required for protein synthesis. AB SCIEX Instruments LC-ESI-MS/MS (Model no. 5068379-Y) QTRAP Enabled Triple Quad 5500+ with Agilent Zorbox C18 (150 mm x 4.6 mm x 3 µm) column and PDA detector was employed for the present study. The total run time was 10 mins and the detection wavelength was 254 nm. A mixture of 5 mM Ammonium formate: Methanol (30: 70) was used as mobile phase on isocratic mode with 1 ml/min as flow rate. Tavaborole has shown linearity over the concentration range 0.5-100 μg/ml and the proposed method was validated as per ICH guidelines. The proposed method is found to be simple, precise, accurate and suitable for the quantification of the marketed formulations of Tavaborole. Stress degradation studies were performed and the method is found to be selective and specific. [ABSTRACT FROM AUTHOR]

Apalutamide is an anti-cancer agent used for the management of prostate cancer. A new stability indicating RP-HPLC method (Gradient mode) has been developed for the estimation of Apalutamide and its related substances using Waters Alliance system (Model no. 2996 and 2695) with Inertsil ODS-3 (250 x 4.6 mm, 5μm) column (PDA detector) was used for the present study. A mixture of Ammonium phosphate buffer solution and Acetonitrile (30: 70, v/v) was used as the mobile phase for the chromatographic study (Flow rate: 1.0 mL/min; Detection wavelength: 243 nm). Stress degradation studies were performed and the method was validated as per ICH guidelines. [ABSTRACT FROM AUTHOR]

Aim: Vildagliptin and Dapagliflozin in fixed-dose combination is used for treatment of Type II Diabetes Mellitus. The key objective of the current research work is to develop a new stability-indicating UHPLC method for the simultaneous estimation of Vildagliptin and Dapagliflozin in tablet dosage form as no such method is available. Materials and Methods: A successful separation was achieved by using Agilent column C18 (4.6×100 mm) and mobile phase of Methanol: 0.1% Orthophosphoric acid (78:22) at a flow rate of 1.0 mL and detection wavelength of 234 nm. The forced degradation study was performed at extreme forced conditions such as hydrolysis with acid and base, peroxide oxidation and photolytic degradation, following ICH guidelines. Results: The retention time for Vildagliptin and Dapagliflozin was 2.3 and 4.7 min respectively. The suggested approach yields linear responses for Vildagliptin and Dapagliflozin in the concentration of the 50-250 µg/mL and 5-25 µg/mL, respectively. Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 1.04 µg/mL and 3.15 µg/mL for Vildagliptin and 0.24 µg/mL and 0.73 µg/mL for Dapagliflozin, respectively. In the exposed conditions, the drugs did not exhibit any significant degradation. Conclusion: The UHPLC approach that was recommended proved to be highly sensitive, accurate, precise, robust and stability indicating. The method can be successfully adopted for the routine analysis for the simultaneous estimation of the Vildagliptin and Dapagliflozin in bulk and pharmaceutical dosage form. [ABSTRACT FROM AUTHOR]

Background and Aim: The current study attempted to invent and evaluate an easy and sensitive Stability indicating UV spectrophotometric method for simultaneous determination of Glimepiride and Pioglitazone HCl. Material and Methods: To provide a simple, sensitive, robust, precise, and accurate Stability indicating UV-Spectrophotometric method for the simultaneous estimate of Glimepiride and Pioglitazone HCl, as well as to develop a combined tablet dosage formulation of Glimepiride and Pioglitazone HCl. The best conditions for drug analysis were found using Methanol as the solvent. Results and Discussion: Glimepiride and Pioglitazone Hydrochloride had maximum absorption wavelengths of 227.6nm and 266.8nm, respectively. Glimepiride and Pioglitazone Hydrochloride demonstrated linear responses between concentration ranges of 2-12g/ml and 5-30g/ml, respectively. It was discovered that the linear regression coefficient was 0.999. According to ICH criteria, the method was validated for sensitivity, specificity, range and linearity, precision, and ruggedness, all validation results were found to be within acceptable limits. Glimepiride and pioglitazone HCl were exposed to forced degradation under ICH guidelines. The resulting samples were used for deterioration experiments utilizing the established procedure. Conclusion: As a result, it may be argued that the procedure was novel, straightforward, precise, specific, and selective for the simultaneous estimation of Glimepiride and Pioglitazone HCl in bulk Drugs. [ABSTRACT FROM AUTHOR]

For the simultaneous determination of anti-hypertensive drugs Hydrochlorothiazide (HCTZ) in bulk and tablet dosage forms, a simple, specific, accurate, and precise stability-indicating UV-Vis Nanodrop 2000c method was developed and validated. The maximum absorption of Hydrochlorothiazide was revealed at 271 nm using methanol as a solvent. The validation results showed good linearity (R2 = 0.9997) within the concentration range of 10-50 µg/mL. The RSD revealed an acceptable value (less than 0.6 percent) in the precision study at three levels. 1.01 and 3.3g µg/mL were found to represent the LOD and LOQ, respectively. Locally and commercial tablets are Available Drug Products. Accuracy at three levels showed good recovery, more than 99% percent. The proposed method was used to analyse the stability of local and commercial tablets. The stability of their pharmaceuticals was investigated under acidic, oxidative, thermal, alkaline, and photolytic conditions in this research. In accordance with the guidelines set by the International Council for Harmonisation (ICH), the method was effectively validated. Subsequently, the validated method was employed to analyze commercially available pharmaceutical dosage forms. [ABSTRACT FROM AUTHOR]

A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF. [ABSTRACT FROM AUTHOR]

Abstract Two rapid, precise, and sensitive stability-indicating high performance chromatographic methods for the measurement of Teriflunomide in its degradation products’ existence were developed. These were RP-HPLC and HPTLC using UV detector. HPLC separation was accomplished utilizing Thermo BDS hypercil C18 column (250 × 4.6 mm, 5 μm) and acetonitrile: 0.03 M potassium dihydrogen phosphate: triethylamine (50:50:0.1%, by volume) as mobile phase at flow rate of 1mL/min. The separated peaks were detected at 250.0 nm. The densitometric approach was conducted utilizing HPTLC 60 F254 silica gel plates, and a developing system of benzene: ethanol: acetic acid (7.5:1:0.25, by volume) and detection was done at 250.0 nm. The developed approaches were evaluated regarding the International Conference on Harmonization (ICH) instructions. The calibration curves of both techniques were constructed with linearity ranges of (5-100) µg/mL and (2–10) µg /band, for HPLC and densitometric determination, consecutively. Teriflunomide was exposed to base and acid hydrolysis, oxidation using H2O2 and finally, thermal degradation as stated in ICH guidelines. The degradation product structures’ elucidation was achieved through LC-MS.

Two rapid, precise, and sensitive stability-indicating high performance chromatographic methods for the measurement of Teriflunomide in its degradation products' existence were developed. These were RP-HPLC and HPTLC using UV detector. HPLC separation was accomplished utilizing Thermo BDS hypercil C18 column (250 × 4.6 mm, 5 μm) and acetonitrile: 0.03 M potassium dihydrogen phosphate: triethylamine (50:50:0.1%, by volume) as mobile phase at flow rate of 1mL/min. The separated peaks were detected at 250.0 nm. The densitometric approach was conducted utilizing HPTLC 60 F254 silica gel plates, and a developing system of benzene: ethanol: acetic acid (7.5:1:0.25, by volume) and detection was done at 250.0 nm. The developed approaches were evaluated regarding the International Conference on Harmonization (ICH) instructions. The calibration curves of both techniques were constructed with linearity ranges of (5-100) µg/mL and (2–10) µg /band, for HPLC and densitometric determination, consecutively. Teriflunomide was exposed to base and acid hydrolysis, oxidation using H2O2 and finally, thermal degradation as stated in ICH guidelines. The degradation product structures' elucidation was achieved through LC-MS. [ABSTRACT FROM AUTHOR]

Background: Teneligliptin is a new drug recently approved by FDA for treatment of type 2 Diabetes Mellitus (DMT 2). Very few methods have been reported for analysing its degradation products and their impact on human health. Materials and Methods: A precise, specific, and sensitive gradient UHPLC technique was developed and validated to analyze Teneligliptin using an Agilent C18 column (4.6x100 mm ID) with 2.5 µm particle size. The method employs a flow rate 0.9 mL/min and detects the teneligliptin at a wavelength 241 nm. This method comprises a mobile phase consists a mixture of Methanol with 0.1% TEA (60:40%v/v), along with a 20 µL injection volume for duration of 20 min. Results: Linearity was found in the range of 2-10 µg/mL having a correlation coefficient of 0.999. The retention time for Teneligliptin was found to be 2.382. Furthermore, the precision and robustness of the method were validated with a remarkable RSD (Relative Standard Deviation) below 2%. Conclusion: The method's stability under various stress conditions was confirmed through forced degradation studies conducted on both bulk substances and pharmaceutical dosage forms. Validation of the method followed the guidelines outlined by the ICH for assessing the validation parameters like specificity, linearity, accuracy, precision, robustness, LOQ and LOD. [ABSTRACT FROM AUTHOR]

A simple, Accurate, precise method was developed for the estimation of the Amantadine in bulk and pharmaceutical dosage form. Chromatogram was run through ACQUITY UPLC BEH C18 Column, 1.7 µm, 2.1 mm X 50 mm. Mobile phase containing 0.1% AmmoniumFormate: Methanol taken in the ratio 73.6 (%v/v) and 26.3 was pumped through column at a flow rate of 0.28 ml/min. Temperature was maintained at 29.21°C. Optimized wavelength selected was ACQUITY TUV ChA 219 nm. Retention time of Amantadine was found to be 1.814 min. %RSD of the Amantadine was found to be 0.4%. %Recovery was obtained as 99.94% for Amantadine. LOD, LOQ values obtained from regression equations of Amantadine were 0.05, 0.15. Regression equation of Amantadine is y = 52995x + 2524.1. with regression coefficient value is found to be 0.99. Retention times were decreased and that run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries. [ABSTRACT FROM AUTHOR]

For the simultaneous determination of anti-hypertensive drugs Hydrochlorothiazide (HCTZ) in bulk and tablet dosage forms, a simple, specific, accurate, and precise stability-indicating UV-Vis Nanodrop 2000c method was developed and validated. The maximum absorption of Hydrochlorothiazide was revealed at 271 nm using methanol as a solvent. The validation results showed good linearity (R2 = 0.9997) within the concentration range of 10-50µg/mL. The RSD revealed an acceptable value (less than 0.6 percent) in the precision study at three levels. 1.01 and 3.3g µg/mL were found to represent the LOD and LOQ, respectively. Locally and commercial tablets are Available Drug Products. Accuracy at three levels showed good recovery, more than 99% percent. The proposed method was used to analyse the stability of local and commercial tablets. The stability of their pharmaceuticals was investigated under acidic, oxidative, thermal, alkaline, and photolytic conditions in this research. In accordance with the guidelines set by the International Council for Harmonisation (ICH), the method was effectively validated. Subsequently, the validated method was employed to analyze commercially available pharmaceutical dosage forms.

This study was motivated by the fact that certain food poisonings and harmful microorganisms in ethanol and water determine roselle (Hibiscus sabdariffa), rosemary (Rosmarinus officinalis), clove (Syzygium aromaticum), and thyme (Thymus vulgaris). is to exhibit the capacity to eliminate Least inhibitory focuses (MICs) of different plant extricates against Gram-positive microorganisms (Bacillus cereus, Staphylococcus aureus), Gram-negative microscopic organisms (Escherichia coli, Enteritidis, Vibrio parahaemolyticus, Pseudomonas aeruginosa) and parasites (Candida albicans) and antibacterial impacts were explored. It is dissolved and measured using the agar well dispersion technique. The concentrate showed antimicrobial efficacy against the microorganisms and yeast used in the tests. Both pHint reduction and cell layer hyperpolarization indicated that the plant extract had a profound effect on the membranes of Gram-positive and Gram-negative microorganisms. Overall, plant extracts have significant potential as unique regular food additives due to their antibacterial properties. [ABSTRACT FROM AUTHOR]

Rivaroxaban is an anticoagulant used to prevent thromboembolism after hip or knee joint replacement surgery. The purpose of study was the development of an efficient, simple and economic reverse phase HPLC-PDA method for Rivaroxaban determination in pharmaceutical dosage forms and blood plasma of human beings. The separation was carried out at room temperature by using Thermo Scientific ODS Hypersil C18 (250×4.6mm, 5µm) and mobile phase 70:30 (%v/v) mixture of ACN / H2O, 1.2 ml/min flow rate, detection on 253nm wavelength by PDA detector with run time of about 7 mins. The retention time observed was about 3 mins. The validation was performed on the proposed method in accordance with ICH guidelines and found that the method is linear within the range of 100-400µg/mL with the correlation coefficient 0.9996. The method was also precise, accurate, robust and rugged, and showed specificity in all applied stress conditions i.e. photolytic (200-800nm, 3h) thermal (70°C, 2h), oxidative (3% H2O2, 70°C, 1h), acidic (0.1 N, 70°C, 1h), and basic (0.1 N, 60°C, 1h). This method was applied successfully for the Rivaroxaban quantitative determination in pharmaceutical dosage and human blood plasma [ABSTRACT FROM AUTHOR]

In this study, an accurate, simple, economical and precise Reversed-Phase High Pressure Liquid Chromatography (RP-HPLC) method was developed for the simultaneous estimation of Ozenoxacin and Benzoic Acid in a pharmaceutical cream formulation, according to the International Conference on Harmonisation (ICH) guidelines. Chromatographic separation was achieved by gradient elution, on RP-HPLC Instrument, equipped with column C8 (150 mm × 4.6 mm, 5 μm particle size) using Ultra Violet (UV) detector at 235 nm wavelength, by using Mobile Phase A: triethylamine, trifloroacetic acid and water (1:1:1000) and Mobile Phase B: methanol and Diluent: water, acetonitrile and triethylamine (500:500:1), at flow rate 0.8 mL min−1; injection volume of 20 μL; column oven temperature 45 °C and sample temperature: 25 °C; Run time: 15 min. All the validation parameters were within the acceptance criteria, as per ICH requirements, for Ozenoxacin and Benzoic acid. Consequently, this method has found to be validated, simple, rapid and successfully applicable, to the simultaneous estimation of Ozenoxacin and Benzoic acid by RP-HPLC, for routine analytical testing in quality control, with a run time of 15 min and for future research studies. Forced degradation of Ozenoxacin cream 1% w/w formulation was performed and found that validated method has stability indicating potential that needs to be further studied. [ABSTRACT FROM AUTHOR]

Eco-friendly liquid chromatographic methods for measuring ergotamine (EGT) are scant in the published database. Accordingly, the goal of the current study was to develop a high-performance thin-layer chromatography (HPTLC) method for fluorescence detection of EGT in commercially available tablets. This approach was based on the application of ethyl alcohol–water (80:20 v/v) as the eco-friendly eluent mixture. The fluorescence detection of EGT was carried out at 322 nm. The greenness score of the present approach was evaluated by "Analytical GREENness (AGREE)" technology. The present approach for measuring EGT in the 25–1000 ng band−1 range was linear. The present assay for fluorescence detection of EGT was validated successfully by ICH guidelines for various parameters. The method was found to be rapid, sensitive, eco-friendly, and stability-indicating. The computed AGREE index for the current strategy was 0.84, displaying outstanding greenness features. The present methodology successfully separated the EGT degradation products under forced-degradation circumstances, exhibiting its stability-indicating qualities and selectivity. An amount of 99.33% of EGT was found in commercial formulations, indicating the validity of the current method for pharmaceutical analysis of EGT in commercial products. The results showed that EGT in commercial products might be regularly measured by the existing method. [ABSTRACT FROM AUTHOR]

Uterine Leiomyomata (commonly known as Fibroids in the uterus) are non-cancerous tumors, most commonly found in women at the premenopausal stage. They are estimated to be found at 33-77% during reproductive age and 70-80% during menopause. The current frontline treatments were ineffective and alternative pharmacological treatments were proposed. Thus, this study aimed at a therapeutic combination of Relugolix, Norethindrone acetate, and Estradiol is proposed. A precise, specific, simple, and selective stability indicating Ultra Performance Liquid Chromatography method for simultaneous determination of the combination has been developed and validated. The chromatographic separation was done by using an isocratic mobile phase of 50:50 v/v acetonitrile and buffer on a phenyl column (100 x 2.1 mm, 1.7 m) with 0.5 ml flow rate/minute, and 272 nm wavelength. The ability of the method to indicate stability was demonstrated by subjecting the Active Pharmaceutical Ingredients to various stressors using appropriate validatory international standard methods. The current study found that the system acceptability (SA), reproducibility (R), detection limits (DL), quantitation limits (QL), linearity (L), accuracy (A), precision (P), and specificity (S) were all within acceptable limits. [ABSTRACT FROM AUTHOR]

Background: Tigecycline (TGC) is a recently developed antibiotic to battle resistant bacteria. The procedures outlined in the literature for analyzing TGC involve chemical solvents that could be hazardous. Therefore, this study aimed to create a sustainable and stable HPLC technique for quantifying Tigecycline in lyophilized powder. The powerful chemometric tool, experimental design (ED), will be applied to analyze the variables' interaction and impact on the selected analytical target profiles. Response surface methodology provides a tutorial on using the central composite design with three levels of variables and quadratic programming to optimize the design space of the developed method. Methods: The New HPLC method consisted of an aqueous buffer and ethanol as a green mobile phase run on a reversed-phase symmetry C18 column. A full resolution between the Tigecycline and its degradation product peaks was achieved in a short analytical runtime. Results: Further, the specificity, accuracy, precision, robustness and stability indicating power of the proposed approach were verified through stress degrading testing. Conclusions: Finally, the analytical eco-scale and the green Analytical Procedure Index (GAPI) were utilized to determine how environmentally friendly the recommended method was compared to other published approaches.

Background: Tigecycline (TGC) is a recently developed antibiotic to battle resistant bacteria. The procedures outlined in the literature for analyzing TGC involve chemical solvents that could be hazardous. Therefore, this study aimed to create a sustainable and stable HPLC technique for quantifying Tigecycline in lyophilized powder. The powerful chemometric tool, experimental design (ED), will be applied to analyze the variables' interaction and impact on the selected analytical target profiles. Response surface methodology provides a tutorial on using the central composite design with three levels of variables and quadratic programming to optimize the design space of the developed method. Methods: The New HPLC method consisted of an aqueous buffer and ethanol as a green mobile phase run on a reversed-phase symmetry C18 column. A full resolution between the Tigecycline and its degradation product peaks was achieved in a short analytical runtime. Results: Further, the specificity, accuracy, precision, robustness and stability indicating power of the proposed approach were verified through stress degrading testing. Conclusions: Finally, the analytical eco-scale and the green Analytical Procedure Index (GAPI) were utilized to determine how environmentally friendly the recommended method was compared to other published approaches.

An efficient, rapid, sensitive, validated stability-indicating ultraviolet spectrophotometric method was developed for flurbiprofen in eye drops. Methanol was employed as the solvent in this proposed process, and detection was carried out at a wavelength of 248 nm. The validation parameters linearity, limit of detection and limit of quantitation, accuracy, precision and specificity were all the subject of experiments according to International Council on Harmonisation guidelines. The stability of flurbiprofen was examined under acidic, alkaline, thermal, and photolytic conditions. The kinetics in the concentration range of 2-10 ug/ml were defined as linear with a correlation value of 0.992. The percentage of relative standard deviation for both intra-day and inter-day accuracy was under less than 2 % and 99.6 %-100.4 % of the drug was retrieved from the study. The system was able to identify variations related to stress conditions although the stress condition of degradation products hadn't been determined. The proposed approach can be employed as a stability indicating method for flurbiprofen screening in conventional pharmaceutical analysis of eye drops with a significant level of linearity, accuracy and precision. The method was found to be both affordable and convenient. This method can therefore be used to study flurbiprofen stress degradation behaviour in small industries without access to sophisticated equipment. [ABSTRACT FROM AUTHOR]

L-Methionine (Met) is an essential alpha-amino acid playing a key role in several metabolic pathways. Rare inherited metabolic diseases such as mutations affecting the MARS1 gene encoding methionine tRNA synthetase (MetRS) can cause severe lung and liver disease before the age of two years. Oral Met therapy has been shown to restore MetRS activity and improve clinical health in children. As a sulfur-containing compound, Met has a strongly unpleasant odor and taste. The objective of this study was to develop an optimized pediatric pharmaceutical formulation of Met powder, to be reconstituted with water, to obtain a stable oral suspension. Organoleptic characteristics and physicochemical stability of the powdered Met formulation and suspension were evaluated at three storage temperatures. Met quantification was assessed by a stability-indicating chromatographic method as well as microbial stability. The use of a specific fruit flavor (e.g., strawberry) with sweeteners (e.g., sucralose) was considered acceptable. No drug loss, pH changes, microbiological growth, or visual changes were observed at 23 ± 2 °C and 4 ± 2 °C with the powder formulation for 92 days, and the reconstituted suspension for at least 45 days. The developed formulation facilitates the preparation, administration, the dose adjustment and palatability of Met treatment in children. [ABSTRACT FROM AUTHOR]

Background: Tigecycline (TGC) is a recently developed antibiotic to battle resistant bacteria. The procedures outlined in the literature for analyzing TGC involve chemical solvents that could be hazardous. Therefore, this study aimed to create a sustainable and stable HPLC technique for quantifying Tigecycline in lyophilized powder. The powerful chemometric tool, experimental design (ED), will be applied to analyze the variables' interaction and impact on the selected analytical target profiles. Response surface methodology provides a tutorial on using the central composite design with three levels of variables and quadratic programming to optimize the design space of the developed method. Methods: The New HPLC method consisted of an aqueous buffer and ethanol as a green mobile phase run on a reversed-phase symmetry C18 column. A full resolution between the Tigecycline and its degradation product peaks was achieved in a short analytical runtime. Results: Further, the specificity, accuracy, precision, robustness and stability indicating power of the proposed approach were verified through stress degrading testing. Conclusions: Finally, the analytical eco-scale and the green Analytical Procedure Index (GAPI) were utilized to determine how environmentally friendly the recommended method was compared to other published approaches.

Abstract Background Tablet dosage forms containing combination of darunavir a protease inhibitor, cobicistat a cytochrome P450 3A inhibitor, emtricitabine and tenofovir alafenamide which were nucleoside reverse transcriptase inhibitors were approved by USFDA on 1st July 2018 to suppress the viral load in HIV patients. It can be used as a complete regimen for the treatment of HIV-1 infection in adults and paediatric patients weighing at least 40 kg. An UPLC method was developed, and separation was done on SB C8 column of dimensions 50 × 2.1 × 1.8 μ with mobile phase 0.01 N potassium dihydrogen ortho phosphate (pH-4.8) and acetonitrile in 60:40 ratio, at a flow rate of 0.3 mL/min and an injection volume of 2 μL. The column temperature was maintained at 30 °C, and detection wavelength was 267 nm. The method was validated according to ICH guidelines. Results The retention times were 1.031, 1.341, 1.630 and 2.153 min, and they were linear in the concentration range of 1.25–7.5 μg/mL, 18.75–112.5 μg/mL, 25–150 μg/mL and 100–600 μg/mL for tenofovir alafenamide, cobicistat, emtricitabine and darunavir, respectively. The intraday and interday precisions were found to be within acceptable limits. LOD was found to be 0.06 μg/mL, 0.51 μg/mL, 1.31 μg/mL and 3.01 μg/mL, and LOQ was 0.19 μg/mL, 1.54 μg/mL, 3.96 μg/mL and 9.13 μg/mL for tenofovir alafenamide, cobicistat, emtricitabine and darunavir. The correlation coefficients were found to be more than 0.999, and recovery was more than 99.52% indicating the method was accurate. Forced degradation studies reveal that the drugs are unstable under acidic conditions. The method was simple, accurate, precise, stable and can be analysed in less runtime of 4 min. Conclusions The flexibility, accuracy and precision of the developed method ensure its applicability in routine analysis of tablet dosage forms. Graphical Abstract

A novel stability-indicating, reversed-phase, high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of favipiravir in an oral suspension. The effective separation of favipiravir and its degradation products was achieved on a Zorbax Eclipse Plus C18 column (5 μm particle size, 150 mm length × 4.6 mm diameter). The mobile phase was prepared by mixing 5 mM of phosphate buffer (pH 3.5) and methanol in a 75:25 v/v ratio delivered at a 1.0 mL/min flow rate. The eluents were monitored using a photodiode array detector at a wavelength of 322 nm. The stability-indicating nature of this method was evaluated by performing force degradation studies under various stress conditions, such as acidic, alkali, oxidative, thermal, and photolytic degradation. Significant degradation was observed during the alkali stress degradation condition. The degradation products generated during various stress conditions were well separated from the favipiravir peak. In addition, the major degradation product formed under alkali stress conditions was identified using UPLC-ESI-TQ-MS/MS and NMR. Method validation was performed according to the ICH Q2 (R1) guideline requirements. The developed method is simple, accurate, robust, and reliable for routine quality control analysis of favipiravir oral suspensions. [ABSTRACT FROM AUTHOR]

Abstract Background A novel gradient, high-sensitive and specific stability-indicating reverse-phase HPLC method was developed and validated for quantitative purpose of known, unknown and degradant impurities profiling for diltiazem hydrochloride tablets. The impurities were separated on the Zorbax RX C8 column (150 mm × 4.6 mm, 5 μm) with mobile phase-A consisting of a mixture of 0.05 M sodium dihydrogen phosphate monohydrate buffer pH 3.0 and methanol in the ratio 800:200v/v and mobile phase-B consisting of acetonitrile with a flow rate of 1.0 mL min−1. The column compartment was maintained at 35 °C, and the detection wavelength was 240 nm. Diltiazem hydrochloride, its known impurities and unknown impurities have been well resolved from each other. Results The linearity of the method has been demonstrated across the concentration range of 0.18 to 5.65 µg mL−1 for EP impurity-F with correlation coefficient R 2 greater than 0.99. Recovery of method was proved from LOQ to 150% for known and unknown impurities with respect to test concentration and found in between 80 and 120%. Forced degradation study and specificity experiment results with mass balance proved the stability-indicating nature of the method and separated all known, unknown impurities and degradants from each other as well as from main drug component (diltiazem hydrochloride). The mass balance for stress study was found in between 95 and 105%. Conclusion Newly developed analytical method was validated as per ICH Q2 (R1) guidelines “Validation of analytical procedure” and found linear, accurate, specific, robust and precise in the established working range.

Abiraterone acetate is an androgen biosynthesis inhibitor used in the treatment of prostate cancer. This study focuses on a simple, economical and systematic liquid-chromatographic and mass spectroscopic method to study the stress degradation behavior of abiraterone acetate under various stress conditions along with its validation. The chromatographic separation of abiraterone acetate and its major degradation product is achieved on Capcell PAK C18 MG-III (100×4.6 mm, 3 µm) column using combination of 0.1 % acetic acid and acetonitrile as mobile phase with a flow rate of 1.2 ml/min and the wavelength of detection is selected as 251 nm. The drug was degraded extensively in acidic and basic hydrolysis. A tentative degradation pathway of drug in acidic and alkaline condition was predicted. The developed analytical method was found selective, accurate, precise and robust in accordance with International Conference on Harmonisation guidelines. The method will also suffice the suitability for the assay of abiraterone acetate in bulk and finished products. [ABSTRACT FROM AUTHOR]

Objectives: A selective, precise and accurate RP-HPLC stability indicating assay method has been developed for the simultaneous estimation of Azilsartan medoxomil and Cilnidipine in tablet dosage form. Materials and Methods: The efficient chromatographic separation of drug was achieved by using C18 (150mm×4.6mm, Agilent 5μm) Column at ambient temperature. Mobile phase contains triethylamine buffer (pH 3.5 adjusted with ortho-phosphoric acid) and acetonitrile (40:60 V/V). Flow rate of mobile phase 1.0 ml/min using isocratic mode. Wavelength selected at 249 nm by using photo diode array detector. Results: The retention time of Azilsartan medoxomil peak 1, Azilsartan medoxomil peak 2 and Cilnidipine were noticed to be 2.16 min, 3.90 min and 9.52 min respectively. The linearity range for Azilsartan medoxomil and Cilnidipine were found to be 50-150 μg/ml and 12.5-37.5 μg/ml and percent recoveries were noticed to be 99.27±0.58 and 98.65±0.49 respectively. Various stress testing conditions such applied to the drug ingredients and drug formulation. The degradants and drugs efficiently separated by using enhanced chromatographic conditions. The developed method was validated as per recommendation parameters of International council on harmonization guideline Q2(R1). Conclusion: The validation parameters stated that the drug substances were efficiently separated from its degradants and developed method can be routinely applied for the simultaneous estimation of Azilsartan medoxomil and Cilnidipine in tablet formulation in a laboratory. [ABSTRACT FROM AUTHOR]

Abstract Background We describe a “stability-indicating liquid chromatography” technique for the estimation of dimethicone (DEC) and dicyclomine hydrochloride (DEH) in the established tablet formulations. Individual quantification of DEH and DEC was reported. But simultaneous quantification of DEH and DEC was lacking. DEH and DEC were analysed on an “XTerra C18 column (250 mm × 4.6 mm, 5 μm)” with the mobile phase solvent run isocratically with 0.1M K2HPO4-acetonitrile (55:45, v/v) on a flow speed of 1.0 mL/min. Results The chromatographic run period for the DEC and DEH assay was 6.0 min with retention times of 2.134 and 2.865 min, respectively. The method was validated for accuracy (99.453 to 100.417% and 99.703 to 100.303% recovery values for DEH and DEC, respectively), precision (RSV value 0.135% for DEC and 0.171% for DEH), linearity (5–15 μg/mL for DEH and 20–60 μg/mL for DEC), selectivity (no hinderance from excipients) and specificity (no hinderance from degradants) recovery. Conclusion The developed stability-indicating liquid chromatography process was well applied to established tablet formulations.

Abstract Background For the determination of gliclazide and its three potential impurities quantitatively, the development of a stability-indicating, accurate, simple, and fast, Ultra-Performance Liquid Chromatography (UPLC) method was done. Results On Acquity CSH 18 column (50 mm×2.1 mm, 1.7 μ) separation was achieved by the isocratic elution mode using mobile phase (5 mM ammonium acetate buffer of pH 4 and 10% ammonium acetate buffer + 90% acetonitrile, 65/35 v/v). In total, 0.7 mL−1 was the chosen flow rate and UV detection was carried out at 227 nm. Conclusion By analyzing forced degradation products of the sample, the stability-indicating characteristic of the developed method was proved where the separation of the products of degradation from analyte peak was seen along with spectral purity of gliclazide. Validation of the developed UPLC method was done as per the guidelines of the International Conference on Harmonization in terms of system suitability, precision, accuracy, specificity, sensitivity, linearity, and robustness.

Abstract Background An easy, defined, rapid, and accurate reverse phase high-performance liquid chromatography method was developed and subsequently validated for the concurrent estimation of lamivudine, efavirenz, and tenofovir disoproxil fumarate in their pure blend and combined tablet formulation. An efficient and appropriate separation of the three analytes was attained with Zorbax eclipse XDB-Phenyl column, with a mobile phase of methanol: buffer (0.1% v/v formic acid in water) (73:27 v/v) at a flow rate of 1mL/min and isocratic elution by using 260nm as detection wavelength. Equal ratio of acetonitrile and water was used as diluent. Results The retention times of lamivudine, tenofovir disoproxil fumarate, and efavirenz were found at 2.6, 4.4, and 5.9 min respectively. The linear response for lamivudine, tenofovir disoproxil fumarate, and efavirenz was in the range of 15.0–45.0μg/mL, 15.0–45.0μg/mL, and 20.0–60.0 μg/mL respectively. The method validation was done in accordance to ICH guidelines and all validation parameters in compliance with ICH standards. The degradants produced by stress testing were well resolved from the peaks of active analytes, which stipulates the stability-indicating property of the method. Conclusion The method has the ability to separate lamivudine, efavirenz, and tenofovir disoproxil fumarate concurrently in blended powder and their combined tablet. All degradants produced by application of stress conditions were separated with high resolution and determined with good sensitivity that ensures the stability-indicating property of the method. Thus, the projected method has high probability to adopt in the pharmaceutical industrial sector.

Abstract Background Most of the analytical methods reported for the estimation of Orlistat were complex, expensive, and deficient in reproducibility with no or very less informative regarding various statistical methods and equations used for the validation purpose. This study provides a fast, accurate, descriptive, and precise isocratic reversed phase high-performance liquid chromatographic (HPLC) method using Waters Spherisorb 5 μm Octadecyl-silica-2 (250 × 4.6 mm) column, for the estimation of Orlistat in bulk drug and pharmaceutical formulations with minimized drug extraction steps. The drug was detected in an analytical column with mobile phase comprising a mixture of methanol, acetonitrile, and 2% phosphoric acid in the ratio of 85:14:1 v/v/v at flow rate of 1 ml/min with elution monitoring at 215.0 nm. Results The retention time for Orlistat was found to be 5.9 min with sharp and proper peak. The linearity was covered over the concentration range of 1.00–10.00 μg/ml (r 2 = 0.9997) with a limit of detection and limit of quantitation 0.06 and 0.2 μg/ml, respectively. The developed analytical technique was found to be validated for all the parameters within the acceptance criteria of ICH guidelines. The mean ± standard deviation (SD) recoveries of Orlistat were 99.87 ± 0.45. Conclusion The optimized method was well precise, accurate, sensitive, stability indicating, and tested with all statistical parameters. Thus, the method can be conveniently used in quality control and routine analysis of Orlistat containing solid dispersions and other formulations. The main advantage of the developed method was its high specificity for the estimation of Orlistat in presence of various degradation products resulting from stress conditions and formulation excipients.

Tripartite synergistic model of solid core technology, dual organic modifiers and combined mixture design was implemented to achieve combined assay and related substances method by reverse phase high performance liquid chromatography with short run time, enhanced sensitivity and improved resolution between multiple impurity peaks. pH of mobile phase, ternary mobile phase composition and high performance liquid chromatography column temperature are experimented as variable parameters. Acetonitrile and isopropyl alcohol mixture was experimented as dual organic modifier. Special focus was given to detailed methodology of dealing with elution order changes by assigning negative sign for resolution. Separation of etoricoxib and related impurities was evaluated as a case study to prove this concept. The method was developed with Ascentis® Express C18, 150×4.6 mm, 2.7 µ column. Mobile phase comprised of buffer (0.1 % v/v ortho phosphoric acid, pH 3.6), acetonitrile and isopropyl alcohol (65.3:29:5.7 v/v) with a flow rate of 1.0 ml/min and ultraviolet detection at 285 nm. Forced degradation studies revealed that the method was stability indicating, suitable for both assay and impurities of drug product. The recoveries for impurities and assay were found to be in the range of 94.0 %-111.0 % and 97.9 %-101.8 %, respectively. Linearity was established for impurities and assay in the range of 0.25-2.0 µg/ml and 125-750 µg/ml, respectively. The method was validated as per international conference on harmonisation guidelines. The method can be successfully employed for determination of assay and impurities of etoricoxib in bulk drugs and formulations. [ABSTRACT FROM AUTHOR]

Quality by Design (QbD) approach was used to facilitate stability indicating HPLC method development of linagliptin (LIN) in tablet dosage form. The method was developed using the PrimesilC18, 250 mm x 4.6 mm, 5µ column using the mobile phase consisting of 0.3% TEA: methanol. (60:40 v/v) pH 4.5 adjusted with o-phosphoric acid. Design of experiment tools was used for optimization of the chromatographic conditions. A three-level Box-Behnken design was employed and statistical analysis of the experimental data showed the significant influential factor of chromatographic conditions. The design space suggested that the current center point parameters could be further modified results with better acceptability for the response parameters. The performance of the optimized method was validated according to ICH guidelines. Linagliptin was exposed to different stress conditions (acid, base, neutral, oxidative, thermal and photolytic) and chromatograms recorded at 292 nm. The degradation of linagliptin followed zero order kinetics for acidic, oxidative and neutral hydrolysis whereas for basic hydrolysis first-order kinetics under experimental conditions. Peak purity plots were evaluated for the degraded sample. The results obtained suggest that the method can be adopted for its analysis and is stability indicating as well. The three-level design helps in understanding the interaction among factors rather than one time one variation as carried out in routine method development. DOI: http://dx.doi.org/10.17807/orbital.v12i2.1194

Abstract Background A Simple, sensitive, and specific stability indicating reverse phase HPLC method was developed for simultaneous estimation of Lamivudine and Dolutegravir in bulk and tablet dosage form. Effective separation was achieved by injecting10 μL of the standard solution into Xbridge Phenyl (250 × 4.6 mm, 5 μ,100 A0) column, using a mobile phase composition of methanol: buffer (0.1% v/v trifluoroacetic acid in water) (85:15 v/v) and isocratic elution programming have been done at a flow rate of 0.8 mL/min. The eluted analytes detected at 258 nm wavelength. The stress conditions such as acid, base, oxidative, thermal, and photo stability were applied as per ICH guidelines to determine the stability of the drugs in different environmental conditions. Results The retention times of Lamivudine and Dolutegravir were found to be 3.4 and 5.0 min respectively. The developed method was linear in the concentration range of 5–15 μg/mL and 30–90 μg/mL for Dolutegravir and Lamivudine respectively. Detection and quantification limits were observed at 3.6 and 11 μg/mL for Lamivudine and 0.50 and 1.5 μg/mL for Dolutegravir. Method validation parameters were within the acceptance criteria of ICH guidelines, and the degradation products were well resolved from Dolutegravir and Lamivudine peaks, which indicate the stability of the method. Conclusion The developed RP-HPLC method was highly precise, specific, sensitive, and stability indicating. Hence, the method has the ability to use in quality control department for regular analysis for the estimation of Lamivudine and Dolutegravir.

Piribedil is a diazinane compound used in the treatment of Parkinson's disease. The objective of the current work was to develop a Quality by design based, stability-indicating high-performance liquid chromatography method, with a short runtime to estimate assay in piribedil prolonged release tablets. The assay is an important critical quality attribute of the drug product, which ensures its efficacy. The critical quality attributes were identified and the quality target method profile was defined. Basis of the initial risk assessment, the separation between piribedil and known/unknown degradation products and the sample preparation procedure's robustness were considered critical factors. Phosphate buffer with 0.01 % triethylamine (pH 2.5; 50 mM) and acetonitrile (80:20, v/v) were used as mobile phase. The peaks were resolved using Hypersil gold C18, (4.6×150) mm, 5 µm column within a runtime of 5 min. The mobile phase was pumped at a flow rate of 1.3 ml/min, whereas the column was maintained at 30°. A 5 µl aliquot of each solution was injected and the peak responses were recorded at 238 nm. The critical chromatographic parameters and sample preparation steps were optimized by using Design of experiments and based on its outcome, method operable design ranges were demarcated. An extensive forced degradation study was executed and all the degradant peaks were well separated from the piribedil peak. Piribedil peak was also found homogenous in all the stressed samples. The developed method was validated and found specific, precise, linear, accurate, rugged and robust. [ABSTRACT FROM AUTHOR]

Background: There is a need for the simple, fast, reliable, economical, specific and sensitivity stability-indicating high performance thin layer chromatographic (HPTLC) method for the estimation of Mometasone furoate (MF) in semi-solid dosage form. Results: The chromatographic separation achieved by using ethyl acetate: acetonitrile: toluene: triethylamine (1.5: 1.5: 7: 0.2 v/v/v/v) as the mobile phase and Rf value was found to be 0.63 at 250nm in UV detection. The developed method is validated according to the ICH guidelines for simplicity, accuracy, precision, detection range, range of magnitude and consistency. The method described is linear with a correlation coefficient (R2)> 0.9992 with a concentration range of 200-1000 ng / band. The recovery was found to be 98.08%. The LOD and LOQ were found to be 36.69 ng / band and 111.18 ng / band respectively. Drug is subject to stress conditions of acid hydrolysis, alkaline hydrolysis, oxidative hydrolysis, neutral hydrolysis, photolysis, thermal degradation. Conclusion: The proposed stability index method can be used to determine the group samples of Mometasone furoate API and pharmaceutical Dosage form. [ABSTRACT FROM AUTHOR]

Background and purpose: Lonidamine is a hexokinase II inhibitor, works as an anticancer molecule, and is extensively explored in clinical trials. Limited information prevails about the stability-indicating methods which could determine the forced degradation of lonidamine under stressed conditions. Hence, we report the use of a rapid, sensitive, reproducible, and highly accurate liquid chromatography and mass spectrometry method to analyze lonidamine degradation. Experimental approach: The Xbridge BEH shield reverse phase C18 column (2.5 μm, 4.6 × 75 mm) using isocratic 50:50 water: acetonitrile with 0.1% formic acid can detect lonidamine with help of mass spectrometer in tandem with an ultraviolet (UV) detector at 260 nm wavelength. Findings/ Results: A linear curve with r2 > 0.99 was obtained for tandem liquid chromatography-mass spectrometry (LC-MS)-UV based detections. This study demonstrated (in the present set up of isocratic elution) that LC-MS based detection has a relatively high sensitivity (S/N (10 ng/mL): 220 and S/N (20 ng/mL): 945) and accuracy at lower detection and quantitation levels, respectively. In addition to developing the LC-MS method, we also report that the current method is stability-indicating and shows that lonidamine gets degraded over time under all three stress conditions; acidic, basic, and oxidative. Conclusion and implications: LC-MS based quantitation of lonidamine proved to be a better method compared to high-performance liquid chromatography (HPLC)-UV detections for mapping lonidamine degradation. This is the first report on the stability-indicating method for studying the forced degradation of lonidamine using LC-MS method.

Background: Ioversol (IVL) is a radiographic contrast agent employed in the diagnostic radiography. In this investigation, our aim was to develop and validate a simple and rapid HPLC-DAD method for determination of IVL in bulk and injection dosage form. Methods: IVL separation and analysis was performed on Zodiac phenyl C18 column (250 mm × 4.5 mm; 5 µ particle size) using water-methanol (90:10 by volume) as mobile phase system and with detection at 254 nm. Results: The retention value of IVL was 4.11 min. The method linearity range was found 254.5-763.5 µg/ml with LOQ and LOD values of 2.376 µg/ml and 0.729 µg/ml, respectively. The accuracy (̴ 100%) and precision (< 2.0%) were within the acceptance criteria. Stability indicating ability of the method was proved by stress degradation studies. Adoptability of this method was assessed with application to marketed injection dosage form with good accuracy (recovery 100.49%) and precision (RSD 0.715%). Conclusion: By adopting this method one can analyze IVL in injection dosage form in less than 10 min and hence this method is time saving and enables the estimation of large number of samples.

Abstract Background Fulvestrant is a new estrogen receptor antagonist available in the market globally for the treatment of hormone receptor-positive metastatic breast cancer in postmenopausal women. Methods The chromatographic separation of fulvestrant was carried out by using ACQUITY UPLC and a BEH Shield RP18, 50 mm × 2.1 mm, i.d 1.7-μm column with a prepared mobile phase consisting of water, acetonitrile, and methanol in the ratio of 300:400:300 (v/v/v), respectively. 1.0 mL orthophosphoric acid was added to the prepared mobile phase. The wavelength for detection was made at 220.0 nm using a PDA-UV detector with a flow rate of 0.3 mL min− 1. Results The system suitability parameters were found within the limits. The coefficient of correlation was found not less than 0.999. The percent recoveries of fulvestrant from 80, 100, to 120% levels are 100.1, 100.4, and 99.7 respectively. The LOD (0.51 μg mL− 1) and LOQ (1.54 μg mL− 1) values from the study demonstrate that the method is sensitive. The samples were subjected to forced degradation conditions of acidic and alkaline hydrolysis, oxidation, photolysis, metallic and thermal degradation in all conditions; peak was found pure (purity angle less than that of threshold). Conclusion A rapid, simple, stability-indicating, and validated RP-UPLC method was developed with 6 min of run time for the quantification of fulvestrant in oil-based injection formulations. This is the first stability-indicating method with the capability of resolving all the fulvestrant degradation impurities in the drug products. The method was validated for system suitability, linearity, precision, accuracy, specificity, intermediate precision, ruggedness, robustness, and solution stability.

The aim and objective of the present work has been to develop new simple, sensitive and validated RP-HPLC method for the estimation of drugs in marketed formulation. Validation of developed Analytical methods according to ICH guidelines. Stress study was performed on Deflazacort and was found that it degrade sufficiently in acidic, alkaline and oxidative condition but less degradation was found in thermal and photolytic oxidation the % of degradation of active constituents was found to be 16.64%, 10.25 %and 8.67% respectively. The analysis was carried out on waters HPLC. It has 715 binary pumps, Rheodyne injector with a 20-microlitre loop, U.V. Vis. Detector, Thermo C-18 column (4.6 x 250mm, 5µ particle size) with data ace software. and the mobile Phase composition was water -methanol ratio 80:20 flow rate 1ml/min, methanol-water ratio 70:30 flow rate 1.2 ml/min, acetonitrile-water ratio 40:60 flow rate 1.2ml/min and methanol - acetonitrile ratio 50:50 fl0w rate 1ml/min at room temperature and most suitable. The sample injection volume was 20 uL, and eluents of the isocratic elution mode were monitored at 241nm. The retention time was 5.25 min. The method was linear in the concentration range of 5-25 ug/ml with an 16.14 r2=0.999. The LOD and LOQ were found to 0.82ug/mL and 2.41ug/mL of Deflazacort. [ABSTRACT FROM AUTHOR]

A nanodrop spectrophotometric method was developed and validated for determination of amlodipine besylate (AB) in bulk and tablet dosage form. The maximum absorption of amlodipine was shown at 357 nm using acetonitrile as a solvent. The developed method was found to be linear (R2 = 0.9990) within the concentration range of 2-10 µg/mL. The precision study showed acceptable values of RSD% (less than 1%). LOD and LOQ values were found to be 0.34 and 1.14 µg/mL, respectively. Accuracy study showed good recovery 99% Awalodipine and 98.88% Amloneer, in locally commercial tablets. The present method was applied successfully for stability indicating study of AB in Awalodipine and Amloneer products manufactured in (Erbil and sulaymaniyah, respectively)/ Kurdistan of Iraq. The stability-indicating study was investigated under acidic, basic, oxidative, photolytic, and thermal conditions. The results of both products showed that AB is unstable in acidic, alkaline, and oxidative conditions under heating at 60℃ up to 5 hrs. While under photolytic and thermal conditions, the degradation percentage was less than 15% indicating to the stability of AB in both Awalodipine and Amloneer tablets according to International Conference on Harmonization (ICH) guideline of drugs. It can be concluded that the main factor that affects the degradation of AB is the passage of time.

A sensitive and accurate stability-indicating spectrofluorimetric method was created and validated for the determination of Cefdinir (CEF), a third-generation cephalosporin drug, via its acid and alkali-induced degradation products. The drug was determined via its acid-induced degradation products at 408 nm using an excitation wavelength of 292 nm, and via its alkali-induced degradation products at 458 nm after excitation at 330 nm. Linearity was achieved in the ranges 0.7–7.0 and 0.03–0.30 μg/mL for the acid-induced and alkali-induced degradation products, respectively. The investigation of degradation pathways was achieved using IR and LC/MS/MS. The technique was also validated by the International Conference on Harmonization Guidelines. The proposed technique was effectively implemented with excellent accuracy and precision to determine CEF in bulk powder and pharmaceutical dosage forms. The final results obtained by the application of the spectrofluorimetric method excellently agreed with the reported HPLC method. [ABSTRACT FROM AUTHOR]

A stability indicating UPLC method has been developed successfully for Hydrocortisone Acetate, Pramoxine Hydrochloride, Potassium Sorbate and Sorbic Acid. The optimized UPLC method can be used for quantitation of Hydrocortisone Acetate, Pramoxine Hydrochloride, Potassium Sorbate and Sorbic acid in finished cream dosage forms. For the estimation of multi components in single method demands more comprehensive way of method development. The optimized UPLC method has been separated all major analytes with optimum resolution. The separation was acquired by using Acquity UPLC BEH column, C18, (150 × 2.1) mm, 1.7 µm particle size and maintained column temp 30 °C. Mobile phase-A contains 10 mM dibasic potassium phosphate (pH of 7.5) and acetonitrile (95: 5 v/v) and mobile phase-B was mixture of acetonitrile and water (90: 10 v/v). The estimation of Hydrocortisone acetate and Sorbate were carried out at 254 nm and for Pramoxine Hydrochloride at 225 nm in PDA detector. The entire chromatographic run time for separation was below 10 min. The curves presented correlation coefficient for three peaks was more than 0.999. Excellent precision and accuracy were obtained for Hydrocortisone acetate, Sorbate and Pramoxine Hydrochloride. Precision and intermediate precision, calculated as relative standard deviation, were lower than 2.2%. Recoveries differed from 97.5% to 102.4%. The drug product was subjected to the different stress conditions as per the current ICH guidelines. The developed stability indicating method approved for quantitative determination of Hydrocortisone Acetate, Pramoxine Hydrochloride, Potassium Sorbate and Sorbic Acid in cream formulations.

Background: Pimavanserin, an antipsychotic agent, is used to treat patients suffering with Parkinson's disease. Till now no stability indicating reverse phase HPLC method was reported for the quantification of pimavanserin in bulk and tablet dosage form. Hence in the present study, a new sensitive, precise and accurate stability indicating reverse phase HPLC method with photodiode array detector has been developed for the quantification of pimavanserin in bulk and tablet dosage form. Methods: Separation and analysis of pimavanserin was achieved on Kromasil C18 (5 µm, 250 mm × 4.6 mm) column using 0.1M NaH2PO4, methanol and acetonitrile in ratio of 55:30:15 (v/v/v) as mobile phase at 25°C. The flow rate was 1.0 ml/min. The effluents were monitored with detector set at 239 nm. The method validation was done with regard to the guidelines by the International Conference on Harmonization. Pimavanserin was subjected to acid, alkali and neutral hydrolysis, hydrogen peroxide oxidation, thermal degradation, and photo (sunlight) degradation. Results: Linear relationship was obtained between the concentration of drug and peak area response in the range of 4.25-34.0 µg/ml. The limits of detection and quantitation were found to be 0.027 µg/ml and 0.089 µg/ml, respectively. All the validation characteristics were within the acceptance criteria. The peaks of degradation products were well resolved from the pimavanserin peak. Conclusion: The developed and validated method is able to quantify the pimavanserin in the presence of degradation products.

A simple, fast, and highly selective RP-HPLC method was developed for the determination of Dapagliflozin (DAP) and Saxagliptin (SAX) in API and tablet dosage form. The separation was done using a Xterra RP18 (4.6×150 mm, 5 μm particle size) column with Acetonitrile: water (60:40). The isocratic elution mode at a flow rate of 1 mL/min, and the analytes were measured at 248 nm. The retention time for DAP and SAX were about 2.091 and 3.249 min, respectively. Calibration curves were found to be linear in the ranges of 100-500 μg/ml for DAP and 50-250 μg/ml for SAX, with correlation coefficients of 0.9998. The detection and quantification values for DAP was 3.0 and 9.98 μg/ml and SAX was 3.02 and 10 μg/ml respectively.