scholarly journals A New Validated Stability Indicating RP-HPLC Method for Simultaneous Quantification of Formoterol Fumarate Dihydrate and Mometasone Furoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (11) ◽  
pp. 2723-2728
Author(s):  
Surya Prakash Mamillapalli ◽  
Gourabattina Lakshmi Prasanna ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Metered Dose ◽  
Formoterol Fumarate ◽  
Dose Inhalation

Stability indicating reversed phase-HPLC method for simultaneous estimation of mometasone furoate (MAF) and formoterol fumarate (FFD) in metered dose inhalation aerosol (MDI) dosage formulation has been developed and discussed in the present work. The chromatographic separation was achieved using Hypersil ODS column (250 mm × 4.6 mm, 3 μm) using an isocratic separation mode at a flow rate of 1.2 mL/min, column temperature of 50 ºC. The system operates with a mobile phase comprising of solution-A (buffer): Solution-B (acetonitrile) mixed in the ratio of 70:30 %v/v at a UV detection wavelength of 214 nm. Retention times of mometasone furoate and formoterol fumarate found to be about 3 min and 7 min, respectively. All possible degradation products of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector. Both analyte were subjected to force degradation studies, found all degradants were resolved from analyte peaks and also other process-related impurities. The proposed method is validated for specificity, linearity, accuracy, precision and robustness as per ICH guidelines and found to be adequate. Method stood to be robust with variation in column temperature, flow rate, pH of buffer and organic content in mobile phase.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Guaifenesin and Dextromethorphan Impurities in Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Thummala V. Raghava Raju ◽  
Noru Anil Kumar ◽  
Seshadri Raja Kumar ◽  
Annarapu Malleswara Reddy ◽  
Nittala Someswara Rao ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
The Stability

A sensitive, stability-indicating gradient RP-HPLC method has been developed for the simultaneous estimation of impurities of Guaifenesin and Dextromethorphan in pharmaceutical formulations. Efficient chromatographic separation was achieved on a Sunfire C18, 250 × 4.6 mm, 5 µm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8 mL min−1 with column temperature of 50°C and detection wavelength at 224 nm. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for Guaifenesin, Dextromethorphan, and their impurities. Guaifenesin and Dextromethorphan formulation sample was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Guaifenesin was found stable and Dextromethorphan was found to degrade significantly in peroxide stress condition. The degradation products were well resolved from Guaifenesin, Dextromethorphan, and their impurities. The peak purity test results confirmed that the Guaifenesin and Dextromethorphan peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness.

scholarly journals Development and validation of stability-indicating RP-HPLC method for the simultaneous estimation of xylometazoline hydrochloride and ipratropium bromide from nasal spray dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Bhaskar Musmade ◽  
Prashant Sanatan ◽  
Surbhi Lokhande ◽  
Shrikant Kulkarni ◽  
Shrinivas Bhope ◽  
...  
Keyword(s):  
Nasal Spray ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Ipratropium Bromide ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Analytical Method Validation ◽  
Development And Validation

Abstract Background A simple, robust, precise, and an accurate HPLC method was established for simultaneous estimation of xylometazoline hydrochloride and ipratropium bromide from a nasal spray dosage form. The effective separation was obtained by injecting 10 μl of sample and standard solutions on to an Inertsil ODS column, 250 × 4.6, mm, 5 μ at 45 °C using phosphate buffer with 1-pentane sulphonic acid sodium salt at pH 4.7 as a mobile phase A and acetonitrile as the mobile phase B. The gradient was optimized with a flow rate of 1 mL/min and a wavelength of 210.0 nm. Result The complete analytical method validation was successfully carried out as per ICH guidelines. The retrieval study was carried out at 50% to 150% level of working concentration, and results were in the range of 99 to 101% for both the analytes. The linearity was proven from 4 to 150% of working concentration with linear regression curve (R2=0.999) for both the analytes. The developed method was robust for different parameters like column temperature, flow rate, mobile phase pH, composition, and gradient. Conclusion The developed HPLC method can be successfully used for the estimation of xylometazoline hydrochloride and ipratropium bromide from nasal spray dosage form as a release test in QC department of manufacturing units.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND AZILSARTAN MEDOXOMIL IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (06) ◽  
pp. 51-61
Author(s):  
J. G Modi ◽  
◽  
J. K. Patel
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Amlodipine Besylate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Azilsartan Medoxomil

A novel, simple, rapid, and highly selective stability indicating RP-HPLC method was developed and validated for simultaneous estimation of azilsartan medoxomil (AZL) and amlodipine besylate HCl (AMLO) in tablet dosage form having strength of 20 mg and 2.5 mg, respectively. The effective chromatographic separation was achieved on a Phenomenex luna ODS C18 (15 cm X 4.6 mm internal diameter, 3.5 μm Particle size) with a mobile phase composed of phosphate buffer (pH-2.5) adjusted with ortho phosphoric acid : acetonitrile in the ratio of 60:40 v/v. The mobile phase was pumped using an isocratic HPLC system at a flow rate of 0.7 mL/min with injection volume 20μl and quantification of the analytes was done at detection wavelength 254 nm. The retention times were found to be 5.918 min and 14.901 min for AMLO and AZL, respectively. The proposed HPLC method was validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, LOD, and LOQ as per ICH Q2 (R1) guideline. Calibration plots were linear over the concentration range of 75-125 µg/mL and 600-1000 µg/mL with correlation coefficients 0.9966 and 0.9948 for AMLO and AZL, respectively. Forced degradation studies were performed using hydrolysis, oxidation, photolytic, and thermal degradation conditions with good resolution between the degradants and analytes. Degradation products resulting from the stress studies did not interfere with the detection of AMLO and AZL, thus the proposed method is sensitive and stability-indicating. The validated HPLC method was successfully applied to the analysis of AMLO and AZL in tablet dosage form.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF BERBERINE AND CURCUMIN IN AN AYURVEDIC FORMULATION

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (08) ◽  
pp. 48-52
Author(s):  
K. P Parekh ◽  
◽  
A. P. Jadhav
Keyword(s):  
Mobile Phase ◽  
Herbal Medicines ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Quality And Safety ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Water Ph ◽  
Development And Validation

A simple, accurate, precise, robust stability indicating RP-HPLC method was developed and validated for simultaneous estimation of berberine and curcumin in an ayurvedic formulation. The two markers were resolved using a C-18 column using as the mobile phase methanol: water (pH 3 adjusted using acetic acid) in the ratio 75:25 V/V at a flow rate of 1mL/min. Retention times of berberine and curcumin were 2.58 ± 0.2 min and 8.5 ± 0.2 min, respectively at 358 nm. Linear response was observed in the concentration range of 2 – 8 ppm for berberine and 5 – 40 ppm for curcumin, with correlation coefficient (r2) of 0.994 and 0.998 for berberine and curcumin, respectively. The developed method was applied for quantitation of markers in marketed and in-house formulations of Gruhadhoomadi Churna. This method can also be used to evaluate formulations containing berberine and curcumin as markers, thus conforming to the need of ensuring quality and safety of herbal medicines.

scholarly journals HPLC method for simultaneous determination of impurities and degradation products in Cardiazol

Pharmacia ◽  
2020 ◽  
Vol 67 (1) ◽  
pp. 29-37
Author(s):  
Iryna Drapak ◽  
Borys Zimenkovsky ◽  
Liudas Ivanauskas ◽  
Ivan Bezruk ◽  
Lina Perekhoda ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Degradation Products ◽  
Phase 1 ◽  
Simultaneous Detection ◽  
Hplc Method ◽  
Column Temperature ◽  
Degree Of Separation ◽  
Determination Of Impurities

Aim. The aim of study was to develop a simple and accurate procedure that could be applied for the determination of impurities and degradation products in cardiazol. Materials and methods. Separation in samples was carried out with Acquity H-class UPLC system (Waters, Milford, USA) equipped with Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) (Waters, Milford, USA). Xevo TQD triple quadrupole mass spectrometer detector (Waters Millford, USA) was used to obtain MS/MS data. Mobile phase A: 0.1% solution of trifluoroacetic acid R in water R; Mobile phase B: acetonitrile R. Samples were chromatographed in gradient mode (Table 1). Flow rate of the mobile phase: 1 ml / min. Column temperature: 30 °С. Detection: at 240 nm wavelength. Injection volume: 10 μl. Results. The retention time of the main substance is about 18.5 minutes. The order of the peak, the retention times and relative retention times: impurity B (12.04, 0.65); impurity А (18.5; 0.98); Cardiazol (18.87; 1.00). The LOD and LOQ values obtained were in the range of 30 ng/mL to 100 ng/mL and 80 ng/mL to 310 ng/mL respectively (with respect to sample concentration of 2 mg/ml). Linearity was established in the range of LOQ level to 0.2% having regression coefficients in the range of 0.9996 to 0.9999. The change in the temperature of the column affects the degree of separation of cardiazol and the impurity A, and thus, with a decrease of 5 ° C, the degree of separation is (1.06), while with increasing this index (3.43). When changing the flow rate of the mobile phase, the degree of separation changes in the following order, with a decrease to 0.9 ml / min separation (1.90), with an increase in speed to 1.1 ml / min (2.45). When the number of mobile phase B decreases by 5%, the degree of separation varies by (2.65), with an increase of 5% (1.82). In comparison with the chromatogram of the tested solution, the substance is not resistant to the action of peroxide, alkaline and acid decomposition. Conclusion. 1) HPLC method was developed and validated for the simultaneous detection and quantitation of impurities formed during the synthesis of cardiazol. 2) The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating.

scholarly journals A New Validated Stability indicating RP-HPLC Method for Simultaneous Quantification of Impurities of Fluticasone Propionate and Salmeterol Xenafoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (4) ◽  
pp. 867-872
Author(s):  
Surya Prakash Mamillapalli ◽  
Shirisha Koyya ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Fluticasone Propionate ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Metered Dose ◽  
Dose Inhalation

A simple, specific, precise, accurate and stability indicating reversed phase HPLC method for simultaneous quantification of total 12 impurities of fluticasone propionate and salmeterol xenafoate in metered dose inhalation aerosol has been developed in the present work. Chromatographic separation between impurities of both compounds were achieved on Altima C18 250 × 4.6 mm, 5 μ column using a step-gradient elution at a flow rate of 1.4 mL/min, 0.1% v/v orthophosphoric acid as buffer and acetonitrile as mobile phase constituents. Forced degradation studies for drug product were performed and revealed that Salmeterol is acid sensitive (about 21.3%), degrades to IMP-D and fluticasone is alkali sensitive (about 7.6%) and degrades to IMP-A. All degradant and process related impurities of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector, which proved stability indicating capability of the method. The developed method is fully validated as per current ICH guidelines, where precision is achieved at % RSD of < 5, Correlation of < 0.999 for linearity, LOD-LOQ at < 0.02% and < 0.05%, along with satisfactory system suitability results under robustness conditions.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

Development and Validation of Stability Indicating HPLC Method for the Simultaneous Estimation of LevocloperastineFendizoate and Chlorpheniramine Maleate in Pharmaceutical Dosage Form

2017 ◽  
Vol 8 (03) ◽  
Author(s):  
Sankalp Patel ◽  
Jinal Tandel ◽  
Samir Shah
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Chlorpheniramine Maleate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Stress Degradation

The aim of the present study was to develop and validate stability indicating HPLC method for simultaneous estimation of LevocloperastineFendizoate (LCP) and Chlorpheniramine Maleate (CPM). HPLC method for simultaneous analysis of both drugs was developed and validated according to ICH guideline. Efficient chromatographic separation was achieved on ODS column C18 (250 mm × 4.6 mm, 5 μm) using the optimized mobile phase. Stability indicating assay method was carried out by different stress degradation conditions. In HPLC method, the Retention time for LCP and CPM was 3.173 min and 5.060 min using optimized mobile phase Phosphate buffer (pH-3.5): Methanol (60:40 %v/v) and UV detection at 273 nm. The degradation of LCP, CPM and Formulation was shown to be highest in alkaline condition. Linearity was observed in concentration range of 20-80 μg/ml for LCP and 4-16 μg/ml for CPM. The correlation coefficient of LCP and CPM were respectively 0.9992 and 0.9994. All validation parameters were within the acceptable range. The LOD and LOQ values for HPLC method were found to be 0.146 μg/ml and 0.444 μg/ml for LCP and 0.0113 μg/ml and 0.0344 μg/ml for CPM respectively. The Method validation parameters showed %RSD value less than 2.

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