scholarly journals A NOVEL ANALYTICAL METHOD FOR SIMULTANEOUS QUANTIFICATION OF DAPAGLIFLOZIN AND SITAGLIPTIN BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2021 ◽  
Vol 10 (3) ◽  
pp. 2861-2865
Author(s):  
Ajay Gupta
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Cost Effective ◽  
Gradient Elution ◽  
Hplc Method ◽  
Reverse Phase ◽  
Simultaneous Quantification ◽  
Validation Parameters

The Reverse phase HPLC method was developed for simultaneous determination of Dapagliflozin and Sitagliptin in single analytical method. Chromatographic separation was achieved on a Hypersil BDS C18 (250mmx4.6mm, 5µm) column applying an gradient elution based on potassium phosphate monobasic buffer pH (3.0) as mobile phase A while methanol and acetonitrile in the ratio of (60:40 v/v) as a mobile phase B with gradient program Time/Mobile phase A%/Mobile phase B% is as 0 min./55/45, 3 min./55/45, 9 min./20/80, 13 min.20/80, 15 min./55/45, 20 min./55/45. Validation parameters specificity, linearity, accuracy, precision and robustness have been observed to be desirable over the concentration ranges of 50-150 µg/ml for Dapagliflozin and Sitagliptin respectively. All the variables have been studied to optimize the chromatographic conditions. The optimized approach verified through validation and confirmed to be the intended purpose for the quality control of the mentioned drugs, as per ICH guidelines. For simultaneous quantification of Dapagliflozin and Sitagliptin, the developed method was found to be genuinely exact precise, accurate, linear, fast, and cost effective.

scholarly journals A Novel Analytical Method for Simultaneous Quantification of Silodosin and Tadalafil by RP-HPLC

2021 ◽  
pp. 193-202
Author(s):  
Ajay Gupta ◽  
S. K. Mishra
Keyword(s):  
Analytical Method ◽  
Potassium Phosphate ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Accuracy Parameter ◽  
Potassium Phosphate Dibasic

The Reverse phase HPLC method was developed for simultaneous determination of Silodosin and Tadalafil in single analytical method. Chromatographic separation was achieved on a Supelco C8 (150mmx4.6mm, 5µm) column applying an isocratic elution based on premix of potassium phosphate dibasic buffer pH (4.3) and acetonitrile in the ratio of (70:30 v/v) as mobile. Validation parameters specificity, precision and robustness have been observed to be desirable over the concentration ranges of 80-240 µg/ml for Silodosin and 50-150 µg/ml for Tadalafil in accuracy parameter and 128-192 µg/ml for Silodosin and 80-120 µg/ml for Tadalafil in linearity parameter. All the variables have been studied to optimize the chromatographic conditions. The optimized approach verified through validation and confirmed to be intended purpose for the quality control of the mentioned drugs, as per ICH guidelines. For simultaneous quantification of Silodosin and Tadalafil, the developed method was found to be genuinely exact precise, accurate, linear, fast and cost effective.

scholarly journals Development and Validation of RP-HPLC Method for Desoximetasone in Bulk and Cream Formulation

2019 ◽  
Vol 9 (3) ◽  
pp. 154-159
Author(s):  
Ashish Gorle ◽  
Jayashri Mahajan ◽  
Prathamesh Bhave
Keyword(s):  
Method Validation ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Topical Steroids ◽  
Cream Formulation ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Development And Validation

Desoximetasone chemically is 9-fluoro-IIβ21-dihydroxy-I6a-methylpregna-I.4-diene-3.The precise mechanism of the anti-inflammatory activity of topical steroids in the treatment of steroid-responsive dermatoses, in general, is uncertain. So, in present investigation chromatographic methods were developing use RP-HPLC for estimation of Desoximetasone in bulk and in cream formulation and method validation according to ICH guidelines. The main objective of this study was to develop a simple and reproducible method for desoximetasone by Reverse Phase High Performance Liquid Chromatography (RP-HPLC). In this work the desoximetasone separation was carried out by using C18 cosmosile column (250mmx4.6mm particle size 5µm). By using 0.1% orthrophosphoric acid pH adjusted up to 3 at uv detection of 240nm.The mobile phase was used at various ratio for gradient elution the ratio of mobile phase was 20:80 v/v. Methanol and water used for mobile phase and flow rate was being set at 1mL/min. The linearity of proposed method was found in range of r =0.9989. Statistically validation parameters such as linearity, accuracy, precision, LOD and LOQ were checked. Keywords: Desoximetasone, RP-HPLC, Method validation.

OPTIMISATION AND VALIDATION OF HPLC METHOD FOR SIMULTANEOUS QUANTIFICATION OF RIFAMPICIN, ISONIAZID, PYRAZINAMIDE, AND ETHAMBUTOL HYDROCHLORIDE IN ANTI-TUBERCULOSIS 4-FDC TABLET

2015 ◽  
Vol 77 (1) ◽  
Author(s):  
Sholihul Khoiri ◽  
Sudibyo Martono ◽  
Abdul Rohman
Keyword(s):  
High Performance ◽  
Phosphate Buffer Solution ◽  
Gradient Elution ◽  
Hplc Method ◽  
Fixed Dose ◽  
Buffer Solution ◽  
Solution Ph ◽  
Combination Tablet ◽  
Simultaneous Quantification ◽  
Dose Combination

High-performance liquid chromatography (HPLC) method has been developed and validated for the simultaneous quantification of four components, namely rifampicin (RIF), isoniazid (INH), pyrazinamide (PYR), and ethambutol hydrochloride (ETM), contained in anti-tuberculosis drugs in fixed dose combination tablet (4-FDC). In order to increase the sensitivity of EMB, the pre-column derivatization technique with phenethyl isocyanate (PEIC) was carried out. The separation was accomplished using Waters Symmetry C8 (250× 4.6 mm i.d.; 5 μm) at 30oC. The mobile phase used was a mixture of acetonitrile and 20 mM phosphate buffer solution (pH 6.8) containing triethylamine and delivered at 1.5 mL/minute using gradient elution. TheUV detector was set at 210 nm. The method was validated in terms of selectivity, linearity, accuracy, precision, detection limit, quantification limit, and robustness according to International Conference on Harmanization (ICH). The optimized method is succcesfully used for quantitative analysis of RIF, INH, PYR and ETM in 4-FDC tablets. The level of these drugs in 4-FDC tablets were in accordance to that specified in Indonesian pharmacopeia.

scholarly journals APPLICATION OF VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF ARMODAFINIL IN BULK AND FORMULATION

2017 ◽  
pp. 158-161
Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Isocratic Mode

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5µ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil. 

scholarly journals Qualitative and quantitative evaluation of melittin in honeybee venom and drug products containing honeybee venom

2013 ◽  
Vol 57 (2) ◽  
pp. 37-44 ◽  
Author(s):  
Ghasem Haghi ◽  
Alireza Hatami ◽  
Mehdi Mehran
Keyword(s):  
High Performance ◽  
Pure Water ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Honeybee Venom ◽  
Drug Products ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Main Component

Abstract A reverse-phase high-performance liquid chromatographic (RP -HPLC ) method was developed and validated for the analysis of honeybee venom samples and drug products containing honeybee venom. The validation parameters were linearity, sensitivity, precision, and recovery. Melittin is the main component of honeybee venom was extracted with pure water, and then evaluated by RP -HPLC with a photodiode array (PDA ) detector. Separation of the samples was achieved on a Europa Protein C18 column with linear gradient elution of acetonitrile and 0.4% phosphoric acid at 25°C. There was a flow rate of 1 mL/min. Detection was set at 220 nm. Limits of detection (LOD ) and quantification (LO Q) for melittin were 1.1 and 3.2 μg/mL, respectively. The amount of melittin in honeybee venom samples ranged from 21.9 to 66.4 %.

scholarly journals Comparative Study on Quantification of Total Catechins Using UV-Vis Spectrophotometric Method and High Performance Liquid Chromatography Techniques

2021 ◽  
Vol 37 (1) ◽  
pp. 136-142
Author(s):  
Sitharanjan Kalidass ◽  
Karuppannau Daiyarvijaya ◽  
Rajagopal Raj Kumar
Keyword(s):  
Quantitative Analysis ◽  
Spectrophotometric Method ◽  
Mobile Phase ◽  
High Performance ◽  
Cost Effective ◽  
Hplc Method ◽  
Good Resolution ◽  
Huge Number ◽  
Automated Hplc

Bioavailability of catechinsin wider range of plants was established earlier and it’s utility as medicine against cardiovascular disease, cancer, etc. were also demonstrated. Recent techniques in relation to quantitative analysis of total catechins seem to be laborious and time consuming process to handle huge number of samples. Established spectrophotometry and HPLC methods developed earlier for quantitative determination of total catechins in tea extracts were compared in the present study.UV-Vis spectrophotometric method was adopted to monitor the absorbance at 500 nm of the reaction mixture (catechins and vanillin-H2SO4reagents). Hewlett Packard automated HPLC was used and equipped with Phenomenex Luna 5  phenyl-hexyl column fitted with a Phenomenex guard column. Binary elution was carried out using Mobile phase A (acetic acid and acetonitrile) and Mobile phase B (acetonitrile). Method adopted showed a good resolution of catechin fractions and was found to be accurate for the quantification of total catechins (sum of individual catechins). Results of the both the methods are comparable and variation amongst the two methods ranged between -3.59 and 2.79% among the clones and varied with seasons.As expected UPASI released tea clones exhibited variations in their bioavailability. Lean season edge over the cropping period sampling in terms of total catechins. Results obtained from both the methods are comparable. Two methods can be used for the routine quantitative analysis of total catechins; however, spectrophotometric method found to be simple, rapid and cost effective than that of HPLC method unless individual catechins composition is warranted.

scholarly journals A Simple Analytical Method for High-Throughput Screening of Major Sugars from Soybean by Normal-Phase HPLC with Evaporative Light Scattering Detection

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Babu Valliyodan ◽  
Haiying Shi ◽  
Henry T. Nguyen
Keyword(s):  
Light Scattering ◽  
Analytical Method ◽  
High Throughput Screening ◽  
Mobile Phase ◽  
High Performance ◽  
Pure Water ◽  
Gradient Elution ◽  
Chromatographic Retention ◽  
Simple Analytical Method ◽  
Evaporative Light Scattering

This paper presents a simple analytical method for determining sugars in soybean (Glycine max (L.) Merr.) tissues. Sample preparation was modified from several early published methods. High-performance liquid chromatography (HPLC) equipped with an evaporative light scattering detector (ELSD) was used to separate, identify, and quantify seven sugars, including glucose, galactose, fructose, sucrose, melibiose, raffinose, and stachyose. Two mobile phases were programed into a gradient elution. Mobile phase A is pure water and mobile phase B is a mixture of acetonitrile and acetone 75 : 25 (v/v). Total chromatographic retention time is less than 20 minutes. This method has been validated for detection limit, calibration range, and intraday and interday repeatability. This method has been used analyzing more than 5000 soybean samples in the experiments studying natural genetic variation of sugar contents and components in soybean seeds and other tissues.

Analytical Method of Gliotoxin Content by HPLC

2012 ◽  
Vol 581-582 ◽  
pp. 46-49
Author(s):  
Xin Qing Zhang ◽  
Ze Ping Xu ◽  
Chuan Lun Yang ◽  
Jian Ping Wang ◽  
Zheng Wei
Keyword(s):  
High Performance Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Mixed Solution ◽  
Determination Method ◽  
Reverse Phase ◽  
Average Recovery ◽  
Reliable Basis

Objective: To establish a determination method for gliotoxin. Methods: Reverse-phase high performance liquid chromatography (HPLC) method was used：the column was Inertsil ODS-SP; detection wavelength set at 254 nm; mixed solution of menthol and water（50:50）was used as the mobile phase with flow rate of 1.0 mL/min. Results: The regression equation of gliotoxin content was y = 9E–08x–0.003. The linear range was 0.5-2.5mg/mL and the average recovery was 99.22%. Conclusion: This method is simple, effective and suitable for analysis of the gliotoxin. A reliable basis was provided for the determination of gliotoxin.

scholarly journals A NOVEL VALIDATED HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC STABILITY-INDICATING ASSAY METHOD IN REVERSE PHASE FOR ESTIMATION OF HYDROXYPROGESTERONE CAPROATE IN AN INJECTABLE FORMULATION.

2021 ◽  
Vol 10 (5) ◽  
pp. 3504-3512
Author(s):  
Vivek Tiwari
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Cost Effective ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Phase Method ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Injectable Formulation ◽  
Liquid Chromatographic

A high-performance liquid chromatographic stability-indicating assay method in reverse-phase has been developed and validated for the quantitative measurement of Hydroxyprogesterone corporate in injectable formulation prepared in castor oil base containing excipient benzyl benzoate as preservative. The reverse-phase method was developed by using Sunfire C18 column having dimensions (150 x 4.6 mm x 5μm) with a mobile phase[A] comprised of water, acetonitrile, and Methanol mixed in 40:30:30 v/v ratio and mobile phase [B] comprised of water, acetonitrile, and Methanol mixed in 20:40:40 v/v ratio pumped gradient program at a flow rate of 1.0 ml/min where the thermostat of the column oven controlled at 30°C and sample compartment at 5°C. The injection volume is set at 20μL. Hydroxyprogesterone corporate has a retention time of 10 minutes with UV detection at 240 nm. The detector was showing linear response in a range of 0.25 μg/ml to 150 μg/ml for Hydroxyprogesterone corporate. The guidelines of the International Conference on Harmonization on guidance for industry (2005) validation of analytical procedures, text, and methodology Q2(R1) were followed for the validation of this novel method. For quantification of Hydroxyprogesterone corporate the developed method was found to be genuinely exact precise, accurate, linear, robust, rugged, stable. and cost-effective.

scholarly journals Development and Validation of Simple, Rapid and Sensitive High- Performance Liquid Chromatographic Method for the Determination of Butenafine Hydrochloride

2020 ◽  
pp. 116-125
Author(s):  
Mohammad Javed Ansari ◽  
Mohammed Muqtader Ahmed ◽  
Md. Khalid Anwer ◽  
Mohammed F. Aldawsari ◽  
Saad M. Al Shahrani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Least Square ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Wide Range

Aims: The current paper reports a simple, rapid, sensitive, accurate, and precise Reverse-phase high performance liquid chromatography (RP-HPLC) method with wide range of estimation to determine butenafine hydrochloride in nanosponges. This method has been validated as per ICH norms. Study Design:  Experimental design with influence of variables such as mobile phase composition, flow rate, temperature and wavelength on the chromatographic peaks. Place and Duration of Study: Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia between Jan 2020 and March 2020. Methodology: Separation was achieved by utilizing the most commonly used reverse phase column (C-18, 5 μm, 150 mm x 4.6 mm) set at 30ºC and quantified by UV detection at 280 nm after isocratic elution from a mobile phase (70:30 v/v of methanol: phosphate buffer pH 3.0) flowing at 1 ml/min. Results: A sharp and symmetrical peak was observed at 4.08 ± 0.01 minutes. The low variation in peak area and retention time (1.12% and 0.29%, respectively) and a high number of theoretical plates (>2000) indicated this method’s efficiency and suitability. The least square linear regression analysis (Y = 9265.5 X + 1961.4) showed excellent correlation (r2 = 0.999 ± 0.0003) between concentration and peak area of butenafine hydrochloride through a wide concentration range of 1–50 µg/ml. The limits of detection and quantification (LOD and LOQ) were 0.18 µg/ml and 0.57 µg/ml, respectively. The assay or determinations were accurate, precise and reproducible with mean accuracy and mean relative standard deviation of precision of 101.53 ± 0.43% and 0.51 ± 0.11% respectively. Conclusion: The developed RP-HPLC method was simple, sensitive, reproducible with wide range of estimation of butenafine hydrochloride in the nanosponges. The proposed method could be used for the analysis of butenafine hydrochloride in the conventional pharmaceutical formulations such as tablets, syrup, creams including novel formulations such as nanoparticles, nanosponges, nanoemulsions. The proposed method overcomes the specificity, sensitivity and reproducibility related issues of ultraviolet-visible spectroscopy.

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