scholarly journals Response Surface Method Aided Development and Validation of Stability Indicating RP-HPLC-UV Method for Impurities of Dextromethorphan Hydrobromide in API and Three Marketed Formulations

2021 ◽  
Vol 33 (11) ◽  
pp. 2737-2745
Author(s):  
Md Irshad Alam ◽  
Aquil-Ur-Rahim Siddiqui
Keyword(s):  
Flow Rate ◽  
Related Compound ◽  
High Performance ◽  
Limit Of Detection ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stress Study ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Dextromethorphan Hydrobromide

An innovative, specific, economical and precise method was developed and validated by employing reverse phase high performance liquid chromatography (HPLC) for contemporaneous estimation of dextromethorphan hydrobromide (DHB) along with its impurities in liquid formulation with forced degradation studies and confirmation of content of DHB in composition label in three market formulations along with their impurities were detected by this method. The optimized chromatographic conditions comprised of column (25 cm × 0.46 cm) × 5 μm Kromasil C8 bearing flow rate of 1.5 mL/min and wavelength 220 nm for UV-estimation. Design of experiments were implemented by following Box Behnken design with most optimum parameters selected as follows, column temperature (A), flow rate (B) and pH (C) with corresponding responses comprised of resolution between related compound A (RCA) and DHB (Y1), tailing of DHB (Y2) and resolution between related compound B (RCB) and DHB (Y3). Stress testing was performed and proved that method was stable as no interfering peaks were observed. All validation parameters including suitability, linearity, accuracy, specificity, limit of detection, limit of quantitation, ruggedness, robustness and stress study were evaluated as per updated ICH guidelines and found to be within limit for pure DHB and detected impurities.

scholarly journals DEVELOPMENT AND VALIDATION OF DAPAGLIFLOZIN BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD AND IT’S FORCED DEGRADATION STUDIES

2017 ◽  
Vol 10 (11) ◽  
pp. 101
Author(s):  
Shaik Shakirbasha ◽  
Sravanthi P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Wave Length ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Column Temperature ◽  
Rp Hplc ◽  
Limit Of Quantitation

  Objective: To develop and validate a simple, selective, precise, and accurate method for the estimation of dapagliflozin using reversed-phase high-performance liquid chromatography (RP-HPLC) technique in bulk and tablet formulation.Methods: The proposed method utilizes chromatographic conditions hypersil BDS (250 mm × 4.6 mm, 5 μ), mobile phase was buffer:acetonitrile (60:40) ratio, flow rate was maintained 1 ml/minute, column temperature was set at 30°C, detection wave length was 245 nm, and diluent was mobile phase.Results: By injecting 5 times of the standard solution system suitability parameters were studied, and results were found well under the acceptance criteria. The linearity study was performed by taking 25-150% levels, and the R2 value was found to be 0.999, precision was found to be 0.5 for repeatability and 0.31 for intermediate precision. The % recovery was found to be 99.89%. Limit of detection and limit of quantitation were found to be 0.60 μg/ml and 1.81 μg/ml, respectively. The % purity was found to be 99.71%. Degradation study on dapagliflozin was performed and concluded that the purity threshold was more than purity angle and within the acceptable range.Conclusion: The developed RP-HPLC method for dapagliflozin was found to be simple, precise, accurate, reproducible, and cost effective. Statistical analysis of the developed method conforms that the proposed method is an appropriate and it can be useful for the routine analysis. This method gives the basic idea to the researcher who is working in area such as product development and finish product testing.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

Method of Validation for Residual Solvents in Bisoprolol Fumarate by GC Technique

2021 ◽  
pp. 147-155
Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Technique ◽  
Range Limit ◽  
Column Temperature ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Chromatographic Condition ◽  
Methylene Dichloride

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were &lt;0.46 and &lt;0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

scholarly journals Development and Validation of Stability-Indicating Reverse Phase-High Performance Liquid Chromatography Method for Simultaneous Determination of Atenolol and Nifedipine in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 219-223
Author(s):  
Ansari Yaasir Ahmed ◽  
Qazi Shoeb ◽  
Umme Rumana ◽  
Patel Afroza ◽  
Pathan Vahid Tajkhan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Limit Of Quantitation

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.

scholarly journals Ultraviolet-Photodiode Array and High-Performance Liquid Chromatographic/Mass Spectrometric Studies on Forced Degradation Behavior of Glibenclamide and Development of a Validated Stability-Indicating Method

2008 ◽  
Vol 91 (4) ◽  
pp. 709-719 ◽  
Author(s):  
Gulshan Bansal ◽  
Manjeet Singh ◽  
Kaur Chand Jindal ◽  
Saranjit Singh
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Mass Spectrometric ◽  
Forced Degradation ◽  
Degradation Behavior ◽  
Prolonged Heating ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

Abstract A forced degradation study on glibenclamide was performed under conditions of hydrolysis, oxidation, dry heat, and photolysis and a high-performance column liquid chromatographic-ultraviolet (HPLC-UV) method was developed to study degradation behavior of the drug under the forced conditions. The degradation products formed under different forced conditions were characterized through isolation and subsequent infrared/nuclear magnetic resonance/mass spectral analyses, or through HPLC/mass spectrometric (HPLC/MS) studies. The drug degraded in 0.1 M HCl and water at 85C toamajor degradation product, 5-chloro-2-methoxy-N-2-(4-sulfamoylphenyl)ethyl]benzamide (III), and to a minor product, 1-cyclohexyl-3-[[4-(2-aminoethyl)-phenyl]sulfonyl]urea (IV). Upon prolonged heating in the acid, the minor product IV disappeared, resulting in formation of 5-chloro-2-methoxy-benzoic acid (II) and an unidentified product (I). Heating of the drug in 0.1 M NaOH at 85C yielded II and IV as the major products and I and III as the minor products. The drug and the degradation products formed under different conditions were optimally resolved on a C18 column using ammonium acetate buffer (0.025 M, pH 3.5)acetonitrile (45 + 55) mobile phase at a flow rate of 0.6 mL/min, with detection at 230 nm. The method was validated for linearity, precision, accuracy, and specificity. Limit of detection (LOD) and limit of quantitation (LOQ) values were also determined. The method could be successfully applied for simultaneous quantification of glibenclamide and the major product, III. The response of the method was linear in a narrow [0.410 g/mL, correlation coefficient (r2 = 0.9982] and a wide (0.4500 g/mL, r2 = 0.9993) concentration range for glibenclamide, and in the concentration range of 0.02550 g/mL (r2 = 0.9998) for III. The method proved to be precise and accurate for both glibenclamide and III. It was specific for the drug and also selective for each degradation product, and LOQ values for the drug were 0.1 and 0.4 g/mL, whereas those for III were 0.010 and 0.025 g/mL, respectively.

RP - HPLC METHOD FOR DETERMINATION OF MEBEVERINE HYDROCHLORIDE IN DOSAGE FORMS EMPLOYING MS COMPATIBLE BUFF ERS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (03) ◽  
pp. 69-72
Author(s):  
Vijaya Lakshmi Marella ◽  
M. Pavani ◽  
Garikapati Devala Raoa
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Life Time ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Quality Control Tool ◽  
Mebeverine Hydrochloride ◽  
Tablet Dosage

A simple, precise, rapid, accurate and economic reverse phase high performance liquid chromatographic method has been developed for the estimation of mebeverine hydrochloride in bulk and tablet dosage form. The separation was achieved by using kinetex column C18 (150×4.6mm, 5µ) and 15mM ammonium acetate and methanol in proportion of 30:70 v/v as mobile phase, at a flow rate of 1.0mL/min. The detection was carried out at 230nm. The retention time of mebeverine was found to be 3.346 minutes.The limit of detection and limit of quantitation were found to be 0.005µg/mL and 0.016µg/mL, respectively. The reliability of the proposed method was ascertained by evaluating various validation parameters like linearity, precision, accuracy and specificity according to ICH guidelines. The proposed method applies LC-MS compatible buffers which increases the life time of column and can be used as lc-ms compatible method. This method acts as a quality control tool for routine analysis of mebeverine hydrochloride in bulk and tablet dosage forms.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

Simultaneous determination of ciprofloxacin hydrochloride and hydrocortisone in ear drops by high performance liquid chromatography

2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Chromatography Method ◽  
Ciprofloxacin Hydrochloride ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Ear Drops

AbstractThe aim of the study was to design and validate a reversed phase high performance liquid chromatography method for the separation and quantification of two active pharmaceutical ingredients (ciprofloxacin hydrochloride, hydrocortisone) and a preservative (benzyl alcohol) in ear drops. Effective separation of the examined compounds was achieved on a GraceSmart™ RP 18 column (150 mm × 4.6 mm, 5 μm) with gradient elution and a diode array detector. The total assay run time was 25 min. Analytical method validation assays were performed. Validation parameters used for the evaluation were: specificity, linearity, trueness, precision (repeatability and reproducibility), limit of detection and limit of quantitation. Results of the validation procedure (high recoveries, good standard deviations, no interfering peaks at the retention times corresponding to the analytes) confirm that the developed chromatographic method can be applied for routine analysis of ear drops.

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

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