scholarly journals Development and validation of HPLC method for the quantification of clotrimazole in a gelatin film formulation

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Surekha Kalshetti ◽  
K. P. Rao
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Gelatin Film ◽  
Average Recovery ◽  
Security Guard ◽  
Ich Guidelines ◽  
System Suitability ◽  
Film Formulation ◽  
Development And Validation ◽  
Separation Of Components

Abstract Background Clotrimazole is used to treat topical vaginal yeast infections. Vaginal gelatin film formulations of clotrimazole were prepared, and the present study aims to develop an HPLC method for quantifying clotrimazole in the film formulation. Results The chromatographic separation of components was achieved on a Phenomenex Luna C18(2) (150 × 4.6 mm, 5 μm) stationary phase with Phenomenex Security Guard Cartridge C18 (4 × 3 mm) using acetonitrile and water (70:30% v/v) as mobile phase. The flow rate was 1.0 ml/min and the absorbance was monitored at 210 nm. Clotrimazole was eluted at 5.6 min. The procedures and capabilities of the method were evaluated against the criteria for system suitability, specificity, linearity, precision, accuracy, and robustness as defined by the ICH guidelines. The method showed good linearity (R2 = 0.999) in the range of 10–50 μg/ml and an average recovery of 101.05%. Conclusion The method could be applied for the quantification of clotrimazole in the gelatin film formulation.

scholarly journals Stability indicating RP-HPLC method for the estimation of flucloxacillin sodium in a tablet dosage form

2020 ◽  
Vol 1 (4) ◽  
pp. 95-100
Author(s):  
Sonalika Patro ◽  
S. Harshith Kumar ◽  
M. Barath kumar ◽  
E. Masthaniah ◽  
K. Sairam ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Theoretical Plate ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Precision Study ◽  
Tablet Dosage

A Simple, accurate and precise method was developed and validated for the determination of flucloxacillin sodium in its tablet dosage form. The separation was eluted on xterra c18 column (4.6x150mm, 5micron) using a mixture of octane buffer and methanol as mobile phase in a ratio of (30:70) which was pumped through column at a flow rate of  1ml/min. Optimised wavelength for flucloxacillin was 237nm, the retention time was 2.305minutes and the percentage purity was found to be 98.14%. System suitability parameters such as theoretical plate and tailing factor for flucloxacillin sodium was found to be 2991.64 and 1.90 respectively, the proposed method was validated as per ICH guidelines (ICH, Q2 AND (R1)) the method was found to be linear at the concentration range of 20-100µg/ml and the correlation coefficient (r2) value was found to be 0.9994 percentage RSD for precision was 0.9% and percentage RSD for ruggedness was 0.5%. The precision study was precise, robust and repeatable. The LOD and LOQ values are 2.98 and 9.98 respectively. Hence the suggested RP-HPLC method can be used for routine analysis for flucloxacillin sodium in tablet dosage form.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Hydroxylamine Hydrochloride content) in Leflunomide by using RP-HPLC technique

2021 ◽  
Vol 37 (02) ◽  
pp. 493-498
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hydroxylamine Hydrochloride ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective, linear having accuracy and specific of reverse phase high-performance liquid chromatographic (RP-HPLC) method for determination of Genotoxic impurity Hydroxylamine Hydrochloride of drug Leflunomide is reported.The separation and analysis were done on YMC Triart C18 (4.6 mm x 150 mm), having particle size 3.0 μm. KH2PO4 in 2000 mL of purified water and 2 mL triethylamine with pH 2.5 with phosphoric acid is mobile phase-A while acetonitrile is mobile Phase-B with gradient program. The elution achieved with 1.50 mL/min flow rate and using UV detection at 230 nm wavelength. Selected column oven temperature is 45°C and auto sampler 5°C respectively. In this method linearity and accuracy of Hydroxylamine HCl covered with specification limit of LOQ to 150 % (i.e.3 to 23 ppm). The observed correlation coefficient is 0.99965 and recovery in between 99.07 to 114.94. In method precision (ie.repeatability) and intermediate precision (IP) observed % RSD of six spiked test preparation is below 5.0 %. The standard and sample were stable for 3 days when stored at 2 to 8°C temperature. In robustness studies system suitability parameters ie tailing factor, theoretical plates and %RSD does not show significant changes. The present RP-HPLC method is selective, robust, linear, and precise for detection of Hydroxylamine HCl.

scholarly journals LC-MS/MS CHARACTERIZATION OF FORCED DEGRADATION PRODUCTS OF TUCATINIB, A NOVEL TYROSINE KINASE INHIBITOR: DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD

2022 ◽  
pp. 58-66
Author(s):  
S. K. REEHANA ◽  
K. SUJANA
Keyword(s):  
Kinase Inhibitor ◽  
Degradation Products ◽  
Degradation Pathway ◽  
Hplc Method ◽  
Forced Degradation ◽  
Ich Guidelines ◽  
System Suitability ◽  
Forced Degradation Studies ◽  
Development And Validation

Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

scholarly journals Method Development and Validation of RP-HPLC Method for the Estimation of Ormeloxifene

2017 ◽  
Vol 2 (03) ◽  
pp. 78-82
Author(s):  
Anusha Shivaraj ◽  
Shireesha Battula
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Isocratic Mode ◽  
Ich Guideline

A new simple, specific, accurate, precise RP-HPLC method has been developed for the estimation of Ormeloxifene. The chromatographic separation for Ormeloxifene was achieved with mobile phase containing methanol :ACN(70:30 v/v), agilent C18 column (4.6 x150 mm) 5 μ at room temperature and UV detection at 274nm.The compounds were eluted in the isocratic mode at a flow rate of 1ml/min. The retention time of Ormeloxifene was found to be 2.497min. The method was validated according to ICH guideline for linearity, specificity, precision, accuracy, LOD, LOQ and robustness in accordance with ICH guidelines.

Development and Validation of Stability Indicating RP-HPLC Method for Estimation of Voriconazole in Bulk Drug

2010 ◽  
Vol 3 (2) ◽  
pp. 978-986
Author(s):  
Wamorkar V V ◽  
C S Ramaa ◽  
Manjunath S Y ◽  
V Malla Reddy
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Good Resolution ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation ◽  
Different Levels

RP-HPLC method has been developed and validated for the determination of voricaonazole in bulk drug. The developed method is found to be specific, reproducible, and stability indicating. The Hypersil, C18 (250 X 4.6 mm) 5μ column was used and mobile phase consisting of water:acetonitrile to achieve good resolution and retention of the analyte and its impurities. The detector linearity was established from concentrations ranging from 5-100 μg/ml. The method was tested at different levels of specificity and accuracy as per requirements given in ICH guidelines. The molecule was exposed to the stress conditions such as acid, base, oxidation, heat and light as per the recommendations of ICH guidelines. The method was proved to be robust with respect to changes in flow rate, mobile phase composition and allied columns. The proposed method is found to be sensitive, precise, rapid, reproducible, and offers good column life.

DEVELOPMENT AND VALIDATION OF RP-HPL C METHOD FOR THE ESTIMATION OF ASCORBIC ACID IN HEALTH DRINKS

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (10) ◽  
pp. 43-47
Author(s):  
N. Mallikarjuna Rao ◽  
◽  
D. Gowri Sankar
Keyword(s):  
Particle Size ◽  
Ascorbic Acid ◽  
Acetic Acid ◽  
Mobile Phase ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Precision And Accuracy ◽  
Development And Validation

A simple, selective, linear, precise and accurate RP-HPLC method was developed and validated for rapid assay of ascorbic acid in health drinks. Isocratic elution at a flow rate of 0.9mL/min was employed on a symmetry C18 column (250x4.6mm, 0.5μ in particle size) at ambient temperature. The mobile phase consisted of water with acetic acid: methanol 95:5% (V/V). The UV detection wavelength was 245 nm and 20μL sample was injected. The retention time for ascorbic acid was 4.61± 0.22 min. The percentage RSD for precision and accuracy of the method was found to be less than the method which was validated as per the ICH guidelines. The method was successfully applied for routine analysis of ascorbic acid in health drinks.

DEVELOPMENT AND VALIDATION OF RP HPLC METHOD FOR THE ESTIMATION OF SOFOSBUVIR IN BULK, TABLET AND INDUSTRIAL WASTE WATER

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (06) ◽  
pp. 59-66
Author(s):  
V Dhanunjayachary ◽  
◽  
V.L.S. Likhitha ◽  
Sri K. Vijaya ◽  
M. A Madhuri
Keyword(s):  
Industrial Waste ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Limit Of Quantitation ◽  
Development And Validation

The study was aimed at development and validation of RP-HPLC method for estimation of sofosbuvir in bulk, pharmaceutical dosage form and pharmaceutical industrial waste. The chromatographic separation was performed on Agilent Syncronis C 18 (100 mm × 4.6 mm, 5μm) column, with a mobile phase comprising of a mixture of methanol: acetonitrile: water (45:30:25 v/v/V). The flow rate was 1.0 mL/min with detection at 260 nm. Retention time of sofosbuvir was found to be 2.040 min. As per ICH guidelines, the method was validated for linearity, accuracy, limit of detection, limit of quantitation, precision, robustness and system suitability. Linearity was found to be in the range of 4-24 μg/mL with regression equation y = 675284.x + 49120 and correlation coefficient 0.999. The low % RSD values indicate the method to be accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.046 and 0.1400 μg/mL, respectively. The % recovery of tablets was found to be in the range of 99.9– 101.3%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for estimation of sofosbuvir in bulk, tablet and applicable for analyses of in pharmaceutical industrial waste.

scholarly journals Development and Validation of RP-HPLC method for Simultaneous Estimation of Metformin and Pioglitazone

2017 ◽  
Vol 5 (01) ◽  
pp. 48-50
Author(s):  
Uttam Kumar Agrawal ◽  
Jeyabalan Govindasamy
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Drug Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A new simple, accurate ,precise and reproducible RP-HPLC method has been developed for simultaneous estimation of metformin and pioglitazone in bulk drug form using proper HPLC system. The mobile phase consists of phosphate buffer and acetonitrile in the ratio of 35:65 at pH 3.4.The detection wavelength was carried out at 228 nm. The method was linear over the concentration range for metformin 50-100 μg/mL and for pioglitazone 20-180 μg/mL. The recoveries of metformin and pioglitazone were found to be 100.5 and 98.7% respectively. The validation of method was carried out utilizing ICH-guidelines. The described HPLC method method was successfully for the analysis of pharmaceutical formulations containing dosage form.

scholarly journals Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

2017 ◽  
Vol 6 (4) ◽  
pp. 133-141 ◽  
Author(s):  
Zampia Tzouganaki ◽  
Michael Koupparis
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Gas Flow ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Development And Validation

In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

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