scholarly journals Simultaneous Determination of Acetaminophen, Pamabrom and Pyrilamine Maleate in Pharmaceutical Formulations Using Stability Indicating HPLC Assay Method

2017 ◽  
Vol 59 (2) ◽  
Author(s):  
Muhammad Ashfaq
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Water Ph

A simple, specific and accurate stability indicating RPHPLC method was developed for the determination of acetaminophen, pamabrom and pyrilamine maleate simultaneously in pharmaceutical dosage forms. Successful separation of all the components was enacted within 10 min using C18 column with mobile phase of methanol and acidified water (pH 1.8) in the ratio of (27: 73 v/v respectively). Flow rate of the mobile phase was 1.5 mL/min with detection at 300 nm. The method was validated in accordance with ICH guidelines. Response was a linear function of concentration over the range of 50- 150 􀈝g/mL for acetaminophen, 2.5-7.5 􀈝g/ mL for pamabrom and 1.5-4.5 􀈝g/mL for pyrilamine maleate. The method resulted in excellent separation of all the analytes along with their stress induced degradation products with acceptable peak tailing and good resolution. It is therefore can be applied successfully for simultaneous determination of acetaminophen, pamabrom and pyrilamine maleate in pharmaceutical formulations and their stability studies.

A Validated Stability-Indicating RP-LC Method for the Simultaneous Determination of Amlodipine and Perindopril in Tablet Dosage Form and Their Stress Degradation Behavior Under ICH-Recommended Stress Conditions

2013 ◽  
Vol 96 (4) ◽  
pp. 751-757 ◽  
Author(s):  
Mehmet Gumustas ◽  
Sibel A Ozkan
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Conditions ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Tablet Dosage

Abstract A stability-indicating RP-LC assay method was developed for the simultaneous determination of the cardiovascular drugs amlodipine and perindopril in the presence of degradation products generated from forced decomposition studies. The developed method is applicable for the determination of related substances in bulk drugs and simultaneous assay in a tablet pharmaceutical dosage form. Separation of the drugs and their degradation products was obtained using an RP Waters Spherisorb ODS1 column (250 × 4.6 mm id, 5 μm particle size) with the mobile phase acetonitrile–water (30 + 70, v/v) containing 15 mM phosphoric acid. The pH of the mobile phase was adjusted to 5.0. A flow rate of 1.2 mL/min was used for the separations, with detection at 215 nm. The chromatographic separation was performed at a column temperature of 45°C. Atenolol was chosen as the internal standard. Amlodipine and perindopril were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation studies showed that both compounds were degraded under these stress conditions. The method was found to be stability-indicating and can be used for the routine analysis of amlodipine and perindopril in the studied combined tablet dosage form.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

scholarly journals Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Uv Light ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Base Temperature ◽  
Stability Indicating ◽  
Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

Stability-Indicating Methods for the Determination of Candesartan Cilexetil in Bulk Drug and Pharmaceutical Formulations

2013 ◽  
Vol 96 (3) ◽  
pp. 580-586 ◽  
Author(s):  
Yousry M Issa ◽  
Emad M Hussien ◽  
Magda M Ibrahim ◽  
Fatma M Abdel-Gawad ◽  
Saadia Barakat
Keyword(s):  
Mobile Phase ◽  
Candesartan Cilexetil ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Stability Indicating ◽  
Bulk Powder ◽  
System Suitability ◽  
The Mean ◽  
Bulk Drug

Abstract Two stability-indicating methods were developed for the determination of candesartan cilexetil in the presence of its degradation products. The first method uses isocratic RP-HPLC with an Agilent C18 column. The mobile phase was phosphate buffer (pH = 2.8 ± 0.1)–acetonitrile (60 + 40, v/v). The flow rate was 2.0 mL/min, and the UV detection was at 254 nm. The second method depends on TLC-densitometric measurements of drug spots at 254 nm. The separation was carried out on silica gel 60 F254 plates using ethyl acetate–methanol–toluene– ammonia 33% (40 + 25 + 20 + 2, v/v/v/v) mobile phase. The methods were validated according to U.S. Pharmacopeia guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, LOD, LOQ, and system suitability were met in all cases. Linear ranges of the methods were 10.0–200.0 μg/mL and 1.0–9.0 μg/spot for HPLC and TLC, respectively. The proposed methods were successfully applied to the drug in bulk powder, in laboratory-prepared mixtures with its degradation products, and in commercially available tablets. The results were compared statistically at the 95% confidence level with each other. There were no significant differences between the mean recovery and precision of the two methods.

scholarly journals Stability Indicating HPLC Determination of Risperidone in Bulk Drug and Pharmaceutical Formulations

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
Navin R. Sheth ◽  
Jigar B. Patel ◽  
Bhavna Patel
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stress Studies ◽  
Liquid Chromatographic Separation ◽  
Bulk Drug ◽  
Liquid Chromatographic

The objective of the current study was to develop a validated stability-indicating assay method (SIAM) for risperidone after subjecting it to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions. The liquid chromatographic separation was achieved isocratically on a symmetry C18 column (5 μm size, 250 mm × 4.6 mm i.d.) using a mobile phase containing methanol: acetonitrile (80 : 20, v/v) at a flow rate of 1 mL/min and UV detection at 280 nm. Retention time of risperidone was found to be . The method was linear over the concentration range of 10–60 μg/mL with a limit of detection and quantitation of 1.79 and 5.44 μg/mL, respectively. The method has the requisite accuracy, specificity, sensitivity, and precision to assay risperidone in bulk form and pharmaceutical dosage forms. Degradation products resulting from the stress studies did not interfere with the detection of Risperidone, and the assay is thus stability indicating.

scholarly journals Development and Validation of a Stability-Indicating Assay Method for Simultaneous Determination of Perindopril and Indapamide in Combined Dosage Form by Reversed-Phase High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (1) ◽  
pp. 108-115 ◽  
Author(s):  
Hitesh Jogia ◽  
Umesh Khandelwal ◽  
Tripti Gandhi ◽  
Sukhdev Singh ◽  
Darshana Modi
Keyword(s):  
Simultaneous Determination ◽  
Stress Testing ◽  
Degradation Products ◽  
Stress Conditions ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Stability Indicating

Abstract An approach of forced degradation study was successfully applied for the development of a stability-indicating assay method for simultaneous determination of perindopril and indapamide in a formulation in the presence of its degradation products. The method showed adequate separation of perindopril and indapamide from their associated main impurities and degradation products. Separation was achieved on an XTerra<sup/> RP18, 5 µm, 150 4.6 mm id column at 55°C by using the mobile phase NaH2PO4 buffer (pH 2.0; 0.005 M)acetonitrile (75 + 25, v/v ) at a flow rate of 1 mL/min and UV detection at 215 nm. Comprehensive stress testing of perindopril and indapamide was carried out according to the International Conference on Harmonization (ICH) guideline Q1A (R2). The specificity of the method was determined by assessing interference from the placebo and by stress testing of the drug (forced degradation). The drug was subjected to acid hydrolysis, base hydrolysis, oxidation, dry heat, and photolysis to apply stress conditions. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method was specific for determination of perindopril and indapamide in the presence of degradation products. The method was validated in terms of linearity, precision, accuracy, specificity, robustness, and solution stability. The linearity of the proposed method was investigated in the range of 2456 µg/mL (r2 = 0.9993) for perindopril and 7.517.5 µg/mL (r2 = 0.9992) for indapamide. Degradation products produced as a result of stress studies did not interfere with the detection of perindopril and indapamide, and the assay can thus be considered stability indicating.

scholarly journals Simultaneous Determination of Diloxanide Furoate and Metronidazole in Presence of Diloxanide Furoate Degradation Products

2011 ◽  
Vol 94 (5) ◽  
pp. 1427-1439
Author(s):  
Samah S Abbas ◽  
Nour E Wagieh ◽  
Mohamed Abdelkawy ◽  
Maha M Abdelrahman
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Principal Component Regression ◽  
Principal Component ◽  
Pharmaceutical Formulations ◽  
Dibasic Potassium Phosphate

Abstract Three methods are presented for the simultaneous determination of diloxanide furoate (DLX) and metronidazole (MTR), used for their antiprotozoal and antiamoebic effect, in the presence of DLX alkaline degradates and in pharmaceutical formulations, without previous separation. The first method is chemometric-assisted spectrophotometry, in which principal component regression and partial least squares were applied. These two approaches were successfully applied to quantify each drug in the mixture using the information included in the absorption spectra in the range of 225–320 nm. The second method is TLC-densitometry, in which the binary mixture and degradates were separated on silica gel plates using a chloroform–acetone–glacial acetic acid (9.5 + 0.5 + 0.07, v/v/v) mobile phase and the bands were scanned at 254 nm. The last method is HPLC, in which DLX, MTR, and degradates were separated using the mobile phase acetonitrile–0.05 M dibasic potassium phosphate (25 + 75, v/v), adjusted to pH 4 with orthophosphoric acid, at a flow rate of 1 mL/min, on a C18 analytical column. Detection was at 254 nm. The proposed methods were successfully applied for the analysis of DLX and MTR in pharmaceutical formulations, and the results were statistically compared with a reported spectrophotometric method.

scholarly journals Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

2013 ◽  
Vol 8 ◽  
pp. ACI.S12478 ◽  
Author(s):  
Ola M. EL-Houssini ◽  
Nagwan H. Zawilla ◽  
Mohammad A. Mohammad
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid ◽  
Development And Validation

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20-200, 20-1000 and 25-1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations.

scholarly journals STABILITY INDICATING RP-LC ASSAY METHOD FOR CARISOPRODOL

2017 ◽  
Vol 9 (6) ◽  
pp. 79
Author(s):  
M. Sangeetha ◽  
Tirumala . ◽  
Nagamallika .
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Hplc Method ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Ich Guidelines ◽  
The Mean

Objective: A reverse phase stability-indicating HPLC method was developed for the determination of Carisoprodol in pharmaceutical dosage forms. The chromatographic elution was achieved on C18, 250 mm × 4.6 mm, 5-μm particle size column.Methods: The mobile phase contains a mixture of water and acetonitrile in ratio of 60:40 v/v. The flow rate was 1.0 ml min-1 and was detected by Refractive index detector.Results: The method was proven to be linear over a range of 1 to 4 mg/ml with a mean correlation coefficient of 0.99998. The %mean recovery is in the range of 100.55% to 101.11% and %RSD was less than 1.0% between preparations. The % RSD for Assay results of initial sample preparation in different intervals of 0hr, 24 h, 30 h and 48 h was less than 1.0%. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from Carisoprodol.Conclusion: The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

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.

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