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.

Development and Validation of Two New Methods for the Determination of Rilmenidine in Bulk and Pharmaceutical Preparation

2021 ◽  
Author(s):  
Elif Özdemir ◽  
Gamze Ergin Kizilçay ◽  
Sıdıka Ertürk Toker
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Gradient Elution ◽  
Hplc Method ◽  
Fluorescence Detector ◽  
New Methods ◽  
Limit Of Quantitation ◽  
Development And Validation

Abstract In the present study, two new methods were developed and validated for the determination of rilmenidine in bulk and pharmaceutical preparation. Both methods are based on a derivatization reaction using 4-chloro-7-nitro-1,2,3-benzoxadiazole (NBD-Cl) as a fluorogenic substance. The drug reagent derivatives were formed by the reaction of rilmenidine with NBD-Cl at pH 9.0 at 70°C for 40 min. The reaction mixtures were analyzed by spectrofluorimetry in the first method and high performance liquid chromatography (HPLC) in the second method. Derivatives were determined at λex 493 nm and at λem 536 nm in the spectrofluorimetric method. The separation was performed place on a Phenomenex, C18 column (250 × 4.6 mm, 5 μm i.d) using a mobile phase comprising 0.2% formic acid and acetonitrile gradient elution mode in the HPLC method. Analytes were detected by a fluorescence detector at the same wavelength. The methods were validated for limit of quantitation, linearity, robustness, recovery, limit of detection, precision and accuracy. Calibration curves for the first and second methods were found to be linear in the range of 2.0–12.0 and 250–2000 ng/mL, respectively. Detection limits for the spectrofluorimetric and HPLC methods were calculated as 0.16 and 18.28 ng/mL, respectively. The validated methods were applied successfully to the determination of rilmenidine in bulk and pharmaceutical preparation.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF LIDOCAINE AND PRILOCAINE IN TOPICAL FORMULATION

2017 ◽  
Vol 10 (10) ◽  
pp. 189
Author(s):  
Narendra M. Gowekar ◽  
Shailesh J Wadher
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Topical Formulation ◽  
Solution Ph ◽  
Column Temperature ◽  
Limit Of Quantitation ◽  
Development And Validation

  Objective: A simple, specific, accurate, and precise method, namely, reverse phase high-performance liquid chromatography was to develop for simultaneous estimation of Lidocaine (LDC) and prilocaine (PLC) in a topical local anesthetic cream.Method: The mixture of PLC and LDC was separated on Hi Q Sil C18 HS column, (250 mm × 4.6 mm, 5 μm), column temperature ambient and flow rate 1.2 mL/minutes. The mobile phase was acetonitrile: 0.01 M diethylamine solution (pH adjusts to 6.8 with orthophosphoric acid) (60:40) with detection at 225 nm.Results: The retention time was found to be 6.075±0.12 minutes for PLC and 8.642±0.15 minutes for LDC, respectively. Linearity was observed in the concentration range of 1-6 μg/mL for both LDC and PLC, respectively. The method was validated according to International Conference on Harmonization guideline and values of linearity, precision, robustness, limit of detection, limit of quantitation, selectivity, and recovery were found to be in good accordance with the prescribed value.Conclusion: The proposed method can be useful in the quality control of LDC and PLC in their topical formulation.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Determination of flavones in species of Thymus L. (Lamiaceae) from Macedonian flora

2001 ◽  
Vol 47 ◽  
pp. 9-14
Author(s):  
Svetlana Kulevanova ◽  
Marina Stefova ◽  
Tatjana Kadifkova Panovska ◽  
Jasmina Tonic ◽  
Trajce Stafilov
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Total Flavonoids ◽  
Column Temperature ◽  
Plant Samples ◽  
Layer Chromatography ◽  
Hydrolysis Of

Assay of flavonoids in extracts of seven Thymus L. (Lamiaceae) species from Macedonia including identification and quantification was performed. Extracts obtained after hydrolysis of air dried samples (A1) were analyzed by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Luteolin and apigenin were identified in comparison to authentic standard substances. The content of total flavonoids in plant samples determined by UV-Vis spectrometry (with AlCl3) ranged from 0.05-0.13 %. Two other extracts were prepared by extraction with a mixture of ethanol:water (7:3, V/V), evaporation until only water remained and extraction first with diethylether (A2) and secondly with ethyl acetate (A3). The content of flavonoids in diethyl-ether and ethyl acetate extracts ranged from 52.5-244.4 mg·ml-1 and 48.7 -117.5 mg·ml-1, respectively. For quantification of luteolin and total flavonoids the HPLC method was applied, using reverse phase column C18, mobile phase consisting of 5% acetic acid and methanol in gradient elution mode and column temperature set to 40 o C. The content of luteolin in the plant samples ranged from 0.23-0.48 % (m/m), while the content of total flavonoids was found to be 0.26-0.52 %.

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.

Sensitive and Fast Determination of Ceftiofur in Honey and Veterinary Formulation by HPLC-UV Method with Pre-column Derivatization

2020 ◽  
Vol 59 (1) ◽  
pp. 15-22
Author(s):  
Noha Rashed ◽  
Sahar Zayed ◽  
Fatma Fouad ◽  
Amany Abdelazeem
Keyword(s):  
Present Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Fast Determination ◽  
Factors Affecting ◽  
Limit Of Quantitation ◽  
Derivatization Reaction

Abstract A novel, sensitive and rapid high performance liquid chromatography (HPLC) method for the determination of ceftiofur by pre-column derivatization with 1,2-naphthoquinone-4-sulfonate. Analysis was performed within 5 min on a Kinetex C18 column based on core-shell technology. The mobile phase composed of acetonitrile-water (50:50, v/v) pumped isocratically at a flow rate of 1.0 mL/min under UV detection at 254 nm. The factors affecting the derivatization reaction and separation conditions were carefully evaluated and optimized. The method was linear over the concentration range of 45–450 ng/mL with a limit of detection of 3.29 ng/mL and limit of quantitation of 10.97 ng/mL. The new method was successfully applied for the analysis of ceftiofur in the veterinary formulation and honey with average recoveries of 100.78% and 98. 83%, respectively. The present method is suitable and favorable for the analysis of ceftiofur on account of its sensitivity, rapidity and cost-effectiveness. In addition, it could have significant application for the determination of ceftiofur in other food products.

scholarly journals Determination of the Contents of Antioxidants and Their Degradation Products in Sodium Chloride Injection for Blood Transfusion

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Bo Tao ◽  
Gang Wang ◽  
Zongning Yin ◽  
Xiaocong Pu ◽  
Yan Jiang ◽  
...  
Keyword(s):  
Sodium Chloride ◽  
Blood Transfusion ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Daily Intake ◽  
Gradient Elution ◽  
Hplc Method ◽  
Polymer Materials ◽  
Limit Of Quantification ◽  
Column Temperature

The infusion bag is mainly made up of polyolefin polymer. Antioxidants are usually added to these polymer materials in the production process to prevent the materials from aging and enhance the stability of the materials. Because of the potential harm of antioxidants to human body, it is necessary to limit the amount of antioxidants migrating to the pharmaceutical solutions. In the present study, we developed and validated the HPLC method for the simultaneous quantification of antioxidants and their degradation products migrating to sodium chloride solution for injection. A total of six antioxidants and six their degradation products were separated and simultaneously determined by using a Waters Symmetry RP18 column (250 × 4.6 mm, 5 μm) and gradient elution of methanol/acetonitrile/acetic acid-water (1 : 99, v/v) at a flow rate of 1.0 mL/min. The detective wavelength was set at 277 nm, and the column temperature was maintained at 35°C. The method was validated in terms of limit of detection (LOD, 0.011–0.151 μg/mL), limit of quantification (LOQ, 0.031–0.393 μg/mL), intraday precision (0.25%–3.17%), interday precision (0.47%–3.48%), linearity (0.1–46.8 μg/mL, r > 0.9994), stability (0.35%–3.29%), and accuracy (80.39%–104.31%). In the extraction experiment, antioxidants, BHT, 1010, 1330, 1076, and 168, and their degradation products, 1310 and DBP, were detected in the packaging materials. Only 1310 was detected in the migration experiment. The maximum daily dosage of sodium chloride for blood transfusion is three bags, and the content of 1310 in long-term testing samples is from 0 to 12 months ranging from 37.44 μg/3 bags to 48.71 μg/3 bags. The daily intake of 1310 did not exceed 48.71 μg, which was much lower than its permitted daily exposure (PDE, 300 μg/day). Therefore, the antioxidants and their degradation products migrating into the drug solution would not cause drug safety risks.

scholarly journals A Simple and Validated Reverse Phase HPLC Methodfor the Determination of Rabeprazole inPharmaceutical Dosage Forms

2010 ◽  
Vol 7 (2) ◽  
pp. 569-577 ◽  
Author(s):  
Uma Mahesh Karra ◽  
Sanjeeva Yarkala
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Tablet Formulations ◽  
Bulk Drug

A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of rabeprazole in bulk drug samples and formulations. Rabeprazole was analyzed by using reverse phase LC-GC column (Inertsil ODS, 4.6 mm x 25 cm, 5 microns), with mobile phase consisting of methanol: water (78:22 v/v). The flow rate was set 1.0 mL/min and analysis was performed at wavelength 288 nm using Photo Diode Array (PDA) detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for rabeprazole was around 4.12 minutes. The calibration curves were linear (r≥0.9998) over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD) and Limit of quantitation (LOQ) were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of rabeprazole in tablet formulations.

scholarly journals Cost Effective, Efficient and Stability indicating Method Development & Validation for determination of related substances for Levonorgestrel & Ethinyl Estradiol Tablets

2021 ◽  
Vol 11 (2) ◽  
pp. 153-163
Author(s):  
Abhiram Dash ◽  
Neelu Jain ◽  
Harish Pandey
Keyword(s):  
Method Validation ◽  
High Performance ◽  
Method Development ◽  
Ethinyl Estradiol ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Hplc Method ◽  
Related Substances ◽  
Limit Of Quantitation

The objective of this research was to develop and validate a simple, specific and accurate reverse phase of high performance of liquid chromatographic method for the determination of levonorgestrel (LVG) and ethinylestradiol (EE) in tablets. The chromatographic system included column Sun Fire ODS (150 mm × 4.6 mm i.d., particle size at 5 μm), mobile phase consisting of acetonitrile: methanol: aquabidest (60:15:25) with the flow rate of 1 mL/minute and effluents monitored at 230 nm. The validation of RP HPLC method for the simultaneous determination of LVG and EE was determined by accuracy, precision, linearity, and limit of detection (LOD) as well as the limit of quantitation (LOQ) parameters. The linearity range of both drugs was 1-70 µg/mL and 2-14 µg/mL for LVG and EE, respectively. The recoveries of LVG and EE were at 101.78% and 102.44% with the coefficients of variation of 0.94% and 1.92%, successively. The LOD of LVG and EE value were of 0.84 µg/mL and 0.03 µg/mL, and LOQ value were of 2.79 and 0.09µg/mL, respectively. Keywords: Levonorgestrel (LVG), Ethinylestradiol, Method Validation, Method Validation, HPLC

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