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.

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.

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.

scholarly journals Simple, Accurate and Efficient High Performance Liquid Chromatographic Method for Determination of Vandetanib in Bulk and in Pharmaceutical Forms

2021 ◽  
pp. 153-160
Author(s):  
M. Murali ◽  
P. Venkateswara Rao
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, linear, precise and accurate isocratic RP-HPLC method was developed and validated for rapid assay of Vandetanib, an anticancer drug, in both bulk and tablet dosage form. Elution at a flow rate of 1ml/min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of acetonitrile, water and orthophosphoric acid in the ratio of 90:08:02 (v/v/v). Linearity was observed in concentration range of 50-200 ppm. The retention time for Vandetanib was 3.326 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Vandetanib in pharmaceutical dosage forms. Moreover the detection alone was also verified through LC-MS of the Vandetanib drug using ESI method which provides future scope for study of this drug using LC-MS method also.

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 Stability-Indicating High-Performance Liquid Chromatographic Determination of Levamisole Hydrochloride in Bulk and Dosage Forms

2020 ◽  
Vol 2020 ◽  
pp. 1-8
Author(s):  
Amal Abdalraheem ◽  
Shaza Shantier ◽  
Imad Abureid ◽  
Elrasheed A. Gadkariem
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Oral Solution ◽  
Official Method ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

A selective, accurate, and precise stability-indicating HPLC method for analysis of levamisole hydrochloride in bulk and in their injection and oral solution formulations has been developed and validated in accordance with ICH guidelines. The chromatographic separation was carried out on a C8 column (250 × 4.6 mm with a particle size of 5 micrometer) using a mixture of phosphate buffer pH 8.0 and acetonitrile (70 : 30 v/v) as the mobile phase pumped at a flow rate of 1.5 ml/min with UV detection at 215 nm. The calibration curve was linear over the 10–50 μg/ml concentration range with a correlation coefficient of 1.0000. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.29 μg/ml and 0.89 μg/ml, respectively. The accuracy and the precision of the developed method were significantly good (RSD < 2%). The validity of the proposed method was further confirmed through the statistical comparison of the obtained data with those of the official method.

scholarly journals A Novel Ultra Performance Liquid Chromatographic Method for the Estimation of Lercanidipine in Bulk and Tablet Dosage Form

2021 ◽  
pp. 768-776
Author(s):  
Satyabrata Sahu ◽  
U. Sunila Kumar Patra ◽  
Pratap Kumar Patra
Keyword(s):  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Ultra Performance Liquid Chromatography ◽  
Stability Study ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Tablet Dosage ◽  
Liquid Chromatographic

Aim: In this present study an accurate reverse phase ultra-performance liquid chromatography (RP-UPLC) method has been developed, validated and applied to stability indicating studies to determine Lercanidipine HCL in bulk and marketed dosage form. Methods: Optimized chromatographic conditions were achieved by using Waters Acquity BEH C18 (2.1 x 50mm, 1.7m) UPLC column. Empower 2 is a software, dihydrogen Orthophosphate Buffer : Methanol (40 : 60)  as eluent at flow rate 0.3 ml/min. PDA detection was performed at 254nm. Results: The developed method was validated and stability study was conducted as per ICH guidelines. The retention time was found at 0.503 min. The method shows linearity over a range of 1 μg/ml to 60 μg /ml with the obtained correlation coefficient is 0.999. The LOD and LOQ values were found 0.025 and 0.05 μg /ml. The acidic and peroxide stressed study shows more degradation of 6.23% and 3.03%. Conclusion: The present developed method was found stability indicating, reliable, validated method was applied for the routine analysis of lercanidipine in bulk drug and the pharmaceutical formulations.

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.

Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Cuminaldehyde

2017 ◽  
Vol 8 (03) ◽  
Author(s):  
Singh Rudra Pratap ◽  
Gangadharappa H. V. ◽  
Narke M. Ramakant ◽  
Jadhav V. Pooja
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Sodium Sulphate ◽  
Herbaceous Plant ◽  
Uv Detector ◽  
Stability Indicating ◽  
Dry Heat ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Limit Of Quantitation

Cumin aldehyde is an herbaceous plant (Cuminumcyminum L.) volatile oil that used as a regular spice in kitchen foods. It also has some pharmacological properties such as analgesic, hepato-protective, anti-inflammatory, antibacterial, antimicrobial, antifungal, antiviral, antioxidant and anticancer. The key objective of the present study was to develop and validate the RP-HPLC method for the estimation of cumin aldehyde. According to the ICH guidelines, RP-HPLC stability indicating method was used in which reverse phase enable Cosmosil C18 column (250 × 4.6 mm, 5μm) used in isocratic mode. For the estimation of cumin aldehyde, sodium sulphate: acetonitrile: methanol (20:73:7 v/v) was used as a mobile phase and it was delivered at flow rate of 1.0 mL min- 1. The injection volume was 20 µL and elute was analyzed by a UV detector at 326 nm. Linearity was observed between the concentration range of 20 μg mL-1 -140 μg mL-1 and the correlation coefficient R2 value was found to be 0.997 ± 0.5. The method was accurate and recovery was found to be in the range of 98.06 -100.40 %. The limit of detection of cumin aldehyde was found to be 1.04 μgmL-1and limit of quantitation was found to be 3.16 μgmL-1. Cumin aldehyde was subjected to stress conditions including acidic, alkaline, neutral, oxidation, and dry heat degradation. Cumin aldehyde was more sensitive to acidic, dry heat and oxidative degradation and it is stable at alkaline conditions. The method was validated according to ICH guidelines.

scholarly journals A Study of Development and Validation of a Method for Simultaneous Estimation of Cidofovir and Famciclovir Using RP-HPLC

2020 ◽  
Vol 11 (4) ◽  
pp. 7878-7884
Author(s):  
Gunturu Raviteja ◽  
Kantipudi Rambabu
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Stability Robustness ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

With the quantitative analysis of Cidofovir and Famciclovir using a Symmetry C-18 150x4.6mm, 3.5 column with a flow rate of 1ml/min, a novel, quick, and accurate high performance liquid chromatographic method have been developed. The buffer is made up of 1 mL formic acid dissolved in 1 litre HPLC water, and the mobile step is made up of a 60:40 mixture of two components: Buffer and Acetonitrile. The detection was done at a wavelength of 250nm. With 8 minutes of run time, the Cidofovir and Famciclovir peaks were split, with the Cidofovir peak eluted at 2.8 minutes and the Famciclovir peak eluted at 6.4 minutes, respectively. In the concentration ranges of 7.5 g/ml to 112.5 g/ml for Cidofovir and 25 g/ml to 375 g/ml for Famciclovir, the proposed method shows strong linearity. The results of the precision and recovery studies range from 98 to 102 percent. The percent RSD in all robustness conditions is less than 2.0 percent. In stressful conditions, deterioration has a limited impact, and solutions remain stable for 24 hours. The parameters of precision, accuracy, specificity, stability, robustness, linearity, limit of detection, and limit of quantification were evaluated and found to be within the appropriate range when the method was developed and validated according to ICH guidelines.

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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