scholarly journals An Ecofriendly and Stability-Indicating HPLC Method for Determination of Permethrin Isomers: Application to Pharmaceutical Analysis

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Minoo Afshar ◽  
Niloufar Salkhordeh ◽  
Mehdi Rajabi
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Phosphoric Acid Solution ◽  
Forced Degradation ◽  
Solution Ph ◽  
Stability Indicating ◽  
Relative Standard

A green, simple, and stability-indicating RP-HPLC method was developed for simultaneous determination of permethrin isomers in pharmaceutical preparations. The separation was based on a C18analytical column (150 × 4.6 mm, i.d., 5 μm). The mobile phase consisted of ethanol: phosphoric acid solution (pH = 3) (67 : 33, v/v). The elution was carried out at 30°C temperature with a flow rate of 1.0 mL/min. Quantitation was achieved with UV detection at 215 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in permethrin concentration range of 0.5–50 μg/mL with correlation coefficients of 0.9996 for each isomer. Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.24%–100.72%) ensured the accuracy of the developed method. The peaks of permethrin isomers well resolved from various degradation products as well as the pharmaceutical excipients. Accordingly, the proposed validated and sustainable procedure was proved to be proper for routine analyzing and stability studies of permethrin in pharmaceutical preparations.

scholarly journals Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Fahimeh Sadeghi ◽  
Latifeh Navidpour ◽  
Sima Bayat ◽  
Minoo Afshar
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Ph ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r2=0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations.

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 Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for Determination of L-Carnitine in Tablets

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Roghaieh Khoshkam ◽  
Minoo Afshar
Keyword(s):  
Hplc Method ◽  
Stability Factor ◽  
Forced Degradation ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Forced Degradation Studies

A rapid and stability-indicating RP-HPLC method was developed for determination of l-carnitine in tablets. The separation was based on a C18 analytical column using a mobile phase which consisted of 0.05 M phosphate buffer (pH = 3): ethanol (99 : 1), including 0.56 mg/mL of sodium 1-heptanesulfonate. Column temperature was set at 50°C and quantitation was achieved by UV detection at 225 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. Among the different stress conditions, the exposure to acidic and basic conditions was found to be an important adverse stability factor. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in l-carnitine concentration range of 84.74–3389.50 µg/mL (r2=0.9997). Precision was evaluated by replicate analysis in which relative standard deviation (RSD) values for areas were found below 2.0%. The recoveries obtained (100.83%–101.54%) ensured the accuracy of the developed method. The expanded uncertainty (3.14%) of the method was also estimated from method validation data. Accordingly, the proposed validated and rapid procedure was proved to be suitable for routine analyzing and stability studies of l-carnitine in tablets.

A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF AZELNIDIPINE AND ITS IMPURITIES IN PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (08) ◽  
pp. 70-76
Author(s):  
Pavani Peddi ◽  
S. L. Tulasi ◽  
N. Usha Rani ◽  
T. Raja Rajeswari
Keyword(s):  
Degradation Products ◽  
Impurity Content ◽  
Hplc Method ◽  
Stability Study ◽  
Forced Degradation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Formulation Analysis

A novel simple, rapid, sensitive and stability-indicating RP-HPLC method was developed and validated for the determination of azelnidipine (ALDP) and its impurities 1 and 2. Resolution of drug, its potential impurities and degradation products were achieved by RP-HPLC on was performed on Prontosil ODS C18 column (250 mm x 4.6 mm, 5µ) using a mobile phase consisting of methanol and 0.1M sodium acetate 40: 60 (v/v) at a flow rate of 1 ml/min and 231 nm of UV detector. Validation of the method was performed along with formulation analysis and forced degradation studies. The calibration curves of ALDP were linear over a concentration range of 50-300 µg/mL. The method was rapid with a retention time of the impurity 2, impurity and ALDP observed at 3.60, 5.15 and 6.90 min, respectively. The method was applied for the impurities determination in drug tablets and for degradation products determination in a stability study of ALDP. The impurity content in the tablets was quantified as 0.1% of total drug. The method can also be used for rapid and accurate quantification of ALDP in its tablets during stability testing.

scholarly journals SEPARATION AND ASSAY OF FOUR ANTIHISTAMINE DRUGS DIPHENHYDRAMINE, CHLORPHENIRAMINE, CYPROHEPTADINE AND FEXOFENADINE IN PHARMACEUTICAL FORMS BY A SINGLE HPLC METHOD

2018 ◽  
Vol 10 (4) ◽  
pp. 53
Author(s):  
Hanan Shasho ◽  
Amir Alhaj Sakur ◽  
Saleh Trefi
Keyword(s):  
Quality Control ◽  
Sulfonic Acid ◽  
Mobile Phase ◽  
Degradation Products ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Deionized Water ◽  
Relative Standard ◽  
Antihistamine Drugs

Objective: The objective of this study was to develop and validate a single HPLC method, in order to separate and assay four antihistamine drugs diphenhydramine, chlorpheniramine, cyproheptadine and fexofenadine in pharmaceutical forms. This method was a practical additional choice in quality control laboratories.Methods: The chromatographic conditions comprised of a classical C18-type stationary phase (150 × 4.6 mm, 5μ), with a mobile phase consisting of, 2.5g of sodium octane sulfonic acid in a mixture of 500 ml of deionized water and 500 ml of acetonitrile, and apparent pH of 2.0 was adjusted with phosphoric acid. The flow rate was 1 ml/min; the detection wavelengths were at 220 nm, 230 nm, 265 nm and 254 nm for diphenhydramine, chlorpheniramine, cyproheptadine and fexofenadine respectively. The temperature was ambient temperature.Results: The method was validated for linearity with correlation coefficients very close to one, the accuracy with mean recovery values between 95.0-105.0%, precision with relative standard deviations of the calculated concentrations less than 5.0% and specificity in the presence of degradation products. Then it was used successfully to separate a mixture of them and to assay these drugs in pharmaceutical forms purchased from Syria.Conclusion: The results presented in this paper showed that the developed method was simple and applicable, for the separation and determination of the four drugs in their pharmaceutical forms.

scholarly journals Stability-indicating RP-HPLC method for determination of beclomethasone dipropionate in nanocapsule suspensions

2015 ◽  
Vol 51 (4) ◽  
pp. 803-810 ◽  
Author(s):  
Janaíne Micheli Chassot ◽  
Luana Mota Ferreira ◽  
Felipe Pereira Gomes ◽  
Letícia Cruz ◽  
Leandro Tasso
Keyword(s):  
Mobile Phase ◽  
Beclomethasone Dipropionate ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Bulk Drug

abstract A simple stability-indicating RP-HPLC/UV method was validated for determination of beclomethasone dipropionate (BD) in nanocapsule suspensions. Chromatographic conditions consisted of a RP C18column (250 mm x 4.60 mm, 5 µm, 110 Å), using methanol and water (85:15 v/v) as mobile phase at 1.0 mL/min with UV detection at 254 nm. The calibration curve was found to be linear in the concentration range of 5.0-25.0 µg/mL with a correlation coefficient > 0.999. Precision was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of BD from nanocapsules (98.03% to 100.35%). Specificity showed no interference from the components of nanocapsules or from the degradation products derived from acid, basic and photolytic conditions. In conclusion, the method is suitable to be applied to assay BD in bulk drug and in nanocapsules, and it can be employed to study stability and degradation kinetics.

scholarly journals Development and validation of the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

scholarly journals Validated Stability-Indicating RP-HPLC Method for the Determination of Norfloxacin in Pharmaceutical Dosage Form

2021 ◽  
Vol 10 (4) ◽  
Author(s):  
Sirajunisa Talath ◽  
Syeda Humaira
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

The objective of this work was to develop a simple, sensitive, accurate, precise and reproducible high performance liquid chromatography (HPLC) method for the determination of norfloxacin in pharmaceutical dosage forms. Shimadzo Prominance model L20 AD HPLC system equipped with SPD 20A UV-Vis detector was used for the analysis. The separation was done on RESTEX allure C18 column (3 μm, 15 cm × 4.6 mm), for an isocratic elution a mixture of methanol and water (60:40, v/v) mobile phase at a wavelength of 254 nm. The flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of norfloxacin was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness as per the ICH guidelines. The retention time of norfloxacin was 7.5 min. The linearity was established over the concentration ranges of 50-350 μg/mL with correlation coefficients ( r2) 0.999.  The percentage accuracy of norfloxacin ranged from 99.76 -101.66%. The relative standard deviation values for intra-day and inter-day precision was lower than 2.0% and the assay result was found to be 100.65 %. Norfloxacin was subjected to stress conditions such as neutral, acidic, alkaline, oxidation and photolysis degradations as per ICH guidelines. The degradation studies revealed that the drug was found to degrade maximum (1.67%) in alkaline degradation conditions and was highly resistant towards neutral, acidic, oxidative and photolytic degradation conditions. Keywords: Norfloxacin, Validation, Stability-indicating, stress degradation, ICH guidelines.  

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