Validated RP-HPLC method for the estimation of Amiloride and hydrochlorothiazide in combined tablet dosage form

2021 ◽  
pp. 207-211
Author(s):  
R. Anantha Kumar ◽  
G. Raveendr Babu ◽  
Sowjanya M. ◽  
Ramayyappa M.
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Tablet Dosage ◽  
Liquid Chromatographic

The aim of this work is to build up a fast, exact, precise and touchy reverse phase liquid chromatographic method for the synchronous assessment of amiloride and hydrochlorothiazide in tablet dose structure. The chromatographic strategy was normalized utilizing Hypersil ODS segment (250×4.6mm, 5μm molecule size) with UV discovery at 210nm and stream pace of 1ml/min. The portable stage includes phosphate buffer (pH acclimated to 2.5 with dilute Ortho Phosphoric acid) and acetonitrile in the proportion of 60:40 v/v. The linearity of proposed technique was examined in the scope of 5-30μg/ml (R²=0.999) for amiloride and 50-300μg/ml (R²=0.999) for Hydrochlorothiazide appropriately. The limit of detection (LOD) was discovered to be 0.10μg/ml and 0.40μg/ml for Amiloride and Hydrochlorothiazide appropriately. The limit of quantitation (LOQ) was discovered to be 0.30μg/ml and 1.20μg/ml for Amiloride and Hydrochlorothiazide separately. The retention times of Amiloride and Hydrochlorothiazide were found to be 3.258min and 2.383min separately. The technique was truly recommended and %RSD was found to be under 2 demonstrating serious level of exactness and accuracy. Subsequently proposed strategy can be effectively evaluated for the synchronous assessment of Amiloride and Hydrochlorothiazide in promoted formulations.

Validated RP-HPLC Method for the Estimation of Amiloride and Hydrochlorothiazide in Combined Tablet Dosage Form

2021 ◽  
pp. 316-320
Author(s):  
R. Anantha Kumar ◽  
G. Raveendra Babu ◽  
Sowjanya M. ◽  
Ramayyappa M.
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Degree Of Exactness ◽  
Phase Liquid ◽  
High Degree ◽  
Tablet Dosage ◽  
Liquid Chromatographic

The aim of this work is to build up a rapid, exact, precise and accurate reverse phase liquid chromatographic method for the simultaneous analysis of amiloride and hydrochlorothiazide in tablet dose structure. The chromatographic strategy was normalized utilizing Hypersil ODS coulmn (250×4.6mm, 5μm molecule size) with UV detection at 210nm and flow rate of 1ml/min. The mobile phase includes phosphate buffer (pH acclimated to 2.5 with dilute Ortho Phosphoric acid) and acetonitrile in the proportion of 60:40 v/v. The linearity of proposed technique was found in the range of 5-30μg/ml (R²=0.999) for amiloride and 50-300μg/ml (R²=0.999) for Hydrochlorothiazide appropriately. The limit of detection (LOD) was discovered to be 0.10μg/ml and 0.40μg/ml for Amiloride and Hydrochlorothiazide appropriately. The limit of quantitation (LOQ) was discovered to be 0.30μg/ml and 1.20μg/ml for Amiloride and Hydrochlorothiazide separately. The retention times of Amiloride and Hydrochlorothiazide were found to be 3.258min and 2.383min separately. The technique was truly recommended and %RSD was found to be under 2 demonstrating high degree of exactness and accuracy. Subsequently proposed strategy can be effectively evaluated for the simultaneous estimation of Amiloride and Hydrochlorothiazide in promoted formulations.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

scholarly journals Development and Validation of a RP-HPLC Method for the Estimation of Amlexanox in Oral Paste Dosage Form

2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

A simple, reproducible and efficient reversed phase high performance liquid chromatographic (RPHPLC) method has been developed for the estimation of a recently approved anti allergic drug, amlexanox in oral paste dosage form. The separations were carried out on a Zorbax Eclipse XBD, C18 column (150 x 4.6 mm; 5?m) at a flow rate of 1.50 ml/min. by using mobile phase comprising of mixed buffer (pH adjusted to 6.50) and methanol (50:50 v/v). The injection volume was 10 ?l and the peaks were detected at 244 nm. The linear dynamic range found to be in the concentration range of 15-35 ?g/ml and coefficient of correlation was found to be 0.999. The %RSD value was below 2.0 for intra-day and inter-day precision which indicated that the method was highly precise. The LOD (Limit of detection) and LOQ (Limit of quantitation) were found to be 3.8 ng/ml and 12.5 ng/ml, respectively which revealed that the method was highly sensitive. The percentage recovery of amlexanox ranged from 99.31 to 99.75%, indicating the accuracy of the method and absence of interference from the excipients present in the formulation. The proposed method was simple, fast, accurate and reproducible and hence can be applied for routine quality control operations of amlexanox in oral paste dosage form. Key words: Amlexanox, Anti allergic, RP-HPLC, LOD, LOQ. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11782 Dhaka Univ. J. Pharm. Sci. 10(2): 67-70, 2011 (December)

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF BAMIFYLLINE HYDROCHLORIDE IN TABLET DOSAGE FORM

2017 ◽  
Vol 9 (4) ◽  
pp. 76
Author(s):  
Panchumarthy Ravisankar ◽  
Shaheem Sulthana ◽  
Inturi Mary Thanuja ◽  
A. Dihitha Chowdary ◽  
J. Vyshnavi
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation ◽  
Tablet Dosage

Objective: The objective of the current study was to develop and validate a novel RP-HPLC method for determination of bamifylline hydrochloride in pharmaceutical dosage form.Methods: Chromatographic separation was conducted on Agilent technologies-1260 series with the G1311C quaternary pump, eclipse XDB C18 column (4.6 mm i.d. X 250 mm, 5 µm particle sizes) and equipped with photodiode array detector G1315D. Mobile phase consisted of methanol and acetonitrile were mixed in the ratio of 90:10 v/v, was used at a flow rate of 1 ml/min and detection wavelength was set at 263 nm.Results: The retention time for bamifylline hydrochloride was found to be 2.913 min. The calibration was linear (r2= 0.9996) in the concentration range of 2-10 µg/ml. The limit of detection and the limit of quantitation were found to be 0.4825 μg/ml and 1.4621 µg/ml respectively. Recovery of bamifylline hydrochloride in tablet formulation was observed in the range of 99.6-99.8 %. Percentage assay of bamifylline hydrochloride (Bamifix) was found to be 99.4 % w/w.Conclusion: Thus the novel proposed method for bamifylline hydrochloride was found to be feasible for the estimation of bamifylline hydrochloride in bulk as well as a pharmaceutical dosage form. 

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OFTRANDOLAPRIL AND VERAPAMIL IN COMBINED TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (05) ◽  
pp. 61-64
Author(s):  
A. L Rao ◽  
◽  
R. V Bhaskara
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A reverse phase high performance liquid chromatographic method was developed and validated asper ICH guidelines for estimation of trandolapril and verapamil in combined tablet dosage form. Theseparation was obtained using a mobile phase consisting of acetonitrile and phosphate buffer adjustingpH to 3.0 in the ratio of 70:30 v/v and using Waters C18 (250 x 4.6 mm, 5 mcm) column maintained atambient temperature. The flow rate was 1.2 mL min-1 and UV detection was monitored at 215 nm. Theretention time (min) and linearity range (mcg mL-1) for trandolapril and verapamil were (5.12, 2.70) and(20-60, 20-60), respectively. The method validation results are within the acceptance criteria for precision,accuracy and linearity. The proposed method was found to be suitable for routine quality control ofmarketed formulation containing these APIs.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND FLUOCINOLONE ACETONIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 134-138
Author(s):  
MADHAVI KUCHANA ◽  
CHAMUNDESWARI KANDUKURU ◽  
PRASANTHI CHENGALVA
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Fluocinolone Acetonide ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation

Objective: To develop and validate a reverse phase high performance liquid chromatographic method for simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on reverse phase Discovery Inertsil ODS3V Column, C18 (250 mm, 4.6 mm, 5 µm). The separation was achieved by employing the mobile phase consists of phosphate buffer (pH 4) and acetonitrile (40:60). The flow rate was 1.0 ml/min, at a detection wavelength of 295 nm. The proposed method was validated as per the International Council for Harmonisation (ICH) guidelines.Results: The retention time for ciprofloxacin and fluocinolone acetonide was found at 3.627 min and 5.037 min respectively. The proposed method was validated for specificity, accuracy, precision, linearity, the limit of detection (LOD), limit of quantitation (LOQ) and robustness. All validation parameters were within the acceptable range. The assay method was linear and found in the range from 12.5–37.25 µg/ml for ciprofloxacin and 0.625–1.875 µg/ml of fluocinolone acetonide. The relative standard deviation (RSD) values for ciprofloxacin and fluocinolone acetonide were 0.25 % and 0.18 %, respectively. Conclusion: A rapid, accurate and precise RP-HPLC method was developed for the simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and ointment formulation. The developed method was validated for specificity, accuracy, precision, linearity, the limit of detection, limit of quantitation and robustness according to ICH guidelines.

scholarly journals Development of Stability Indicating, Validated Liquid Chromatographic Method for Estimation of Sarecycline in its Formulations

2019 ◽  
Vol 35 (6) ◽  
pp. 1805-1812
Author(s):  
Azmath Unissa ◽  
Anupama Koneru ◽  
M. Mushraff Ali Khan ◽  
Murali Balaram Varanasi ◽  
Imam Pasha Syed
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Indicating ◽  
Stability Robustness ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A stability indicating HPLC method was developed and for the estimation of Sarecycline Hydrochloride in tablet dosage form using C18 column with a mobile phase composition of 0.1M Na2PO4 and Acetonitrile in the ratio of 50:50 v/v . The detection wave maxima and retention time were found to 242nm and 3.876min respectively. The method validation was carried out according to International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful estimation of Sarecycline in the pharmaceutical dosage formulations.

scholarly journals DETERMINATION AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF MIRABEGRON IN TABLET DOSAGE FORM

2017 ◽  
pp. 140-151 ◽  
Author(s):  
B. Mounika ◽  
L. Srikanth ◽  
A. Venkatesha
Keyword(s):  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Tablet Dosage

Objective: A reversed phase liquid chromatography was determined and validated for the estimation of Mirabegron in tablet dosage form.Methods: The validation study of RP-HPLC showed a simple, rapid, accurate, precise, reproducible results by using a stationary phase: Waters Acquity HSS T-3 C18 (100 × 2.1 mm, 1.7μm and Mobile Phase-Potassium di-hydrogen phosphate: acetone in the ratio (40:60 v/v) at PH6.0±0.02. Detection is carried out at 243 nm using UV detector.Results: The total chromatographic analysis time per sample was about 6 min with Mirabegron eluting at a retention time of 2.754. Tailing factor obtained from the standard injection is 1.6. Theoretical Plates obtained from the standard injection is 2736.7. The flow rate is 1 ml/min and linearity in the concentration range of 30-70μg/ml (R2=0.999). The precision was 0.4% the intermediate precision was 0.08%. The deliberately varied chromatographic conditions in the concentration range for the evaluation of robustness is 10-50 µg/ml, (n=3). The limit of detection (LOD) and limit of quantitation (LOQ) for Mirabegron were 0.01µg/ml and 0.05µg/ml respectively. The % recovery is 99.8 % with % R. SD of 0.09. The results proved that the optimized HPLC method fulfills these requirements within the ICH accepted limits.Conclusion: The high recovery and low relative standard deviation confirm the suitability of the proposed method for the determination of Mirabegron in tablet dosage form. 

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Simultaneous Estimation of Dapagliflozin Propanediol and Metformin Hydrochloride in Tablet Dosage Form

2020 ◽  
pp. 660-667
Author(s):  
Nikita Shaileshbhai Patel ◽  
Bhavesh Hirabhai Patel
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Tablet Dosage

A rapid, precise, accurate, specific and simple stability indicating RP-HPLC method was developed for simultaneous estimation of Dapagliflozin Propanediol (DAPA) and Metformin Hydrochloride (MET) in its tablet dosage form. Method was performed on a column C8 Thermoquest, hypersil division of dimension 250 mm × 4.60 mm having particle size 5 micron. The mobile phase used in the method was 10 mM Ammonium Acetate buffer (pH- 4), Methanol and Acetonitrile in proportion of 30:65:05 respectively. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, range, precision, accuracy, robustness, LOD, LOQ and system suitability. The flow rate was maintained at 0.8 ml/ min and effluent was monitored at 227 nm. The retention time were observed 5.988 min and 4.661 min for DAPA and MET respectively.  The standard curve was found linear over range of 60-140 μg/ml for DAPA and 300-700 μg/ml for MET with correlation coefficient of 0.9996 for DAPA and 0.9994 for MET. The limit of Detection (LOD) of this method was 1.121 μg/ml for DAPA and 6.162 μg/ml for MET. The limit of Quantitation (LOQ) of this method was 3.396 μg/ml for DAPA and 18.674 μg/ml for MET.  The percentage recovery was found to be in the range of 98-102% at three different levels of a standard addition. The precision (repeatability, intra-day and inter-day) of the method was within the limit (RSD<2%). Degradation products produced because of stress studies did not interfere with the detection of DAPA and MET and the assay can thus be considered stability-indicating. Combination tablet was successfully analysed using the developed method.

scholarly journals Development of Simple and Robust RP-HPLC Method for Determination of Everolimus and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantitation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.

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