scholarly journals An HPLC method for the determination of digoxin in dissolution samples

2010 ◽  
Vol 75 (11) ◽  
pp. 1583-1594 ◽  
Author(s):  
Miroslav Milenkovic ◽  
Valentina Marinkovic ◽  
Predrag Sibinovic ◽  
Radosav Palic ◽  
Dragan Milenovic
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Stability Testing ◽  
Column Length ◽  
Column Temperature ◽  
Chromatographic Parameters ◽  
The Impact ◽  
Full Factorial ◽  
Phase Column

An HPLC method for digoxin quantification in dissolution samples obtained as per the official British Pharmacopeia (BP) method is presented in this paper. The chromatography was performed at 20 ?C on a Symmetry C18; 3.5 ?m, 75 x 4.6 mm column with water - acetonitrile (72 : 28, v/v), as the mobile phase and UV detection at 220 nm. The method was found to be selective, linear, accurate and precise in the specified ranges. The LOD and LOQ were 0.015 ?g mL-1 and 0.050 ?g mL-1, respectively. Robustness testing was conducted to evaluate the impact of minor changes in the chromatographic parameters (i.e., acetonitrile fraction, flow rate of the mobile phase, column temperature and column length) on the characteristics of the digoxin peak. A. full factorial design (24) was used to investigate the influence of the four variables The presented HPLC method was applied in quality and stability testing of Digoxin tablets 0.25 mg.

scholarly journals DETERMINATION OF 2-CYANO-4’-BROMOMETHYL BIPHENYL GENOTOXIC IMPURITY IN IRBESARTAN DRUG SUBSTANCES USING HPLC TECHNIQUE

2016 ◽  
Vol 8 (12) ◽  
pp. 225
Author(s):  
S. Senthil Kumar ◽  
Ritesh Kumar Srivastava ◽  
V. Srinivas Rao
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Development Activity ◽  
Validation Data ◽  
Column Temperature ◽  
Injection Volume ◽  
Drug Substances ◽  
Hplc Technique ◽  
Ich Guideline

<p><strong>Objective: </strong>The objective of present study was to develop and validate a specific and sensitive HPLC method for the quantitative determination of genotoxic impurity 2-cyano-4’-bromomethyl biphenyl present in irbesartan drug substance.</p><p><strong>Methods: </strong>The development activity was conducted by HPLC with UV as a detector. The impurity was separated on Kromasil C18 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of buffer pH 3.2 and acetonitrile in the ratio of 60:40 v/v at a flow rate 1.5 ml/min. The effluent was monitored by UV detection at 258 nm with column temperature maintained at 40 °C and the injection volume 30 μl. Acetonitrile was selected as diluent.</p><p><strong>Results: </strong>Validation activity was planned and completed based on the ICH guideline. The LOD and LOQ value were found to be 0.167 µg/g and 0.506 µg/g and accuracy results were well in the range 98.34 to 103.46 %. The linearity curve showed the correlation coefficient of 0.9999 and method very sensitive.</p><p><strong>Conclusion: </strong>From validation data, it was confirmed that the developed method is specific, sensitive, linear, precise and accurate for the determination of 2-cyano-4’-bromomethyl biphenyl genotoxic impurity in irbesartan drug substances.</p>

scholarly journals ISOLATION, CHARACTERIZATION AND VALIDATION OF HPLC METHOD FOR QUANTIFICATION OF BIS-[10-(2-METHYL-4H-3-THIA-4,9-DIAZABENZO[F]AZULENE)]-1,4-PIPERAZINE IN AN ANTI-PSYCHOTIC DRUG SUBSTANCE, OLANZAPINE

2018 ◽  
Vol 10 (4) ◽  
pp. 22
Author(s):  
Suresh Babu Bodempudi ◽  
Ravi Chandra Babu Rupakula ◽  
Konda S. Reddy ◽  
Mahesh Reddy Ghanta
Keyword(s):  
Mobile Phase ◽  
Sodium Hydroxide Solution ◽  
Linear Regression Analysis ◽  
Sodium Dodecyl ◽  
Hplc Method ◽  
Drug Substance ◽  
Phase System ◽  
Column Temperature ◽  
Relative Standard

Objective: The main objective of present study was to Isolate, characterize and validate a reverse phase high performance liquid chromatographic method was validated for quantification of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance; it decreases the mental disorders in human body. The method is specific, rapid, precise and accurate for the separation and determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance form.Methods: The bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of Olanzapine was resolved on a Zorbax RX-C 8, 250 mm X 4.6 mm, 5 micron column (L-1) using a mobile phase system containing 0.03 M sodium dodecyl sulphate in water pH 2.5 with 1 N sodium hydroxide solution and acetonitrile in the ratio of (Mobile phase A-52:48 v/v) and (Mobile phase B-buffer and Acetonitrile 30:70 v/v) by using the gradient program. The mobile phase was set at a flow rate of 1.5 ml/min and the volume injected was 20μl for every injection. The detection wavelength was set at 220 nm and the column temperature was set at 35 °C.Results: The proposed method was productively applied for the quantitative determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo [f]azulene)]-1,4-piperazine in Olanzapine drug substance form. The linear regression analysis data for calibration plots showed a good linear relationship over a concentration range of 0.025to 0.903 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine, 0.081-0.608 µg/ml for Olanzapine. The mean values of the correlation coefficient were 0.999 and 0.999 for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The method was validated as per the ICH guidelines. The detection limit (LOD) was about 0.007 µg/ml, 0.024 µg/ml and quantitation limit (LOQ) was about 0.024 µg/ml, 0.081 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The relative standard deviation was found to be 1.64 % and 2.18 % for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine.Conclusion: The validated HPLC method and the statistical analysis showed that the method is repeatable and selective for the estimation of the bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of the Olanzapine drug substance.

scholarly journals Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities

2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Stability Testing ◽  
Stability Indicating ◽  
Chromatographic Parameters ◽  
Interday Precision ◽  
Calculated Amount

Abstract A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was &lt;1 and &lt;1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of &gt;2 from the nearest peak. Insignificant changes in retention time (&lt;4) and calculated amount (&lt;1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.

scholarly journals HPLC method for simultaneous determination of impurities and degradation products in Cardiazol

Pharmacia ◽  
2020 ◽  
Vol 67 (1) ◽  
pp. 29-37
Author(s):  
Iryna Drapak ◽  
Borys Zimenkovsky ◽  
Liudas Ivanauskas ◽  
Ivan Bezruk ◽  
Lina Perekhoda ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Degradation Products ◽  
Phase 1 ◽  
Simultaneous Detection ◽  
Hplc Method ◽  
Column Temperature ◽  
Degree Of Separation ◽  
Determination Of Impurities

Aim. The aim of study was to develop a simple and accurate procedure that could be applied for the determination of impurities and degradation products in cardiazol. Materials and methods. Separation in samples was carried out with Acquity H-class UPLC system (Waters, Milford, USA) equipped with Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) (Waters, Milford, USA). Xevo TQD triple quadrupole mass spectrometer detector (Waters Millford, USA) was used to obtain MS/MS data. Mobile phase A: 0.1% solution of trifluoroacetic acid R in water R; Mobile phase B: acetonitrile R. Samples were chromatographed in gradient mode (Table 1). Flow rate of the mobile phase: 1 ml / min. Column temperature: 30 °С. Detection: at 240 nm wavelength. Injection volume: 10 μl. Results. The retention time of the main substance is about 18.5 minutes. The order of the peak, the retention times and relative retention times: impurity B (12.04, 0.65); impurity А (18.5; 0.98); Cardiazol (18.87; 1.00). The LOD and LOQ values obtained were in the range of 30 ng/mL to 100 ng/mL and 80 ng/mL to 310 ng/mL respectively (with respect to sample concentration of 2 mg/ml). Linearity was established in the range of LOQ level to 0.2% having regression coefficients in the range of 0.9996 to 0.9999. The change in the temperature of the column affects the degree of separation of cardiazol and the impurity A, and thus, with a decrease of 5 ° C, the degree of separation is (1.06), while with increasing this index (3.43). When changing the flow rate of the mobile phase, the degree of separation changes in the following order, with a decrease to 0.9 ml / min separation (1.90), with an increase in speed to 1.1 ml / min (2.45). When the number of mobile phase B decreases by 5%, the degree of separation varies by (2.65), with an increase of 5% (1.82). In comparison with the chromatogram of the tested solution, the substance is not resistant to the action of peroxide, alkaline and acid decomposition. Conclusion. 1) HPLC method was developed and validated for the simultaneous detection and quantitation of impurities formed during the synthesis of cardiazol. 2) The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

scholarly journals Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities

2013 ◽  
Vol 63 (2) ◽  
pp. 159-173 ◽  
Author(s):  
Irena Kasagić ◽  
Anđelija Malenović ◽  
Marko Jovanović ◽  
Tijana Rakić ◽  
Biljana Jančić Stojanović ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Fractional Factorial ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature ◽  
Rp Hplc ◽  
Temperature Separation ◽  
Validation Parameters ◽  
Water Ph ◽  
Chromatographic Parameters

This paper presents the chemometrically assisted optimization and validation of the RP-HPLC method intended for the quantitative analysis of itraconazole and its impurities in pharmaceutical dosage forms. To reach the desired chromatographic resolution with a limited number of experiments in a minimum amount of time, Box- -Behnken design was used to simultaneously optimize some important chromatographic parameters, such as the acetonitrile content in the mobile phase, pH of the aqueous phase and the column temperature. Separation between itraconazole and impurity F was identified as critical and selected as a response during the optimization. The set optimal mobile phase composition was acetonitrile/ water pH 2.5 adjusted with o-phosphoric acid (50:50, V/V). Separations were performed on a Zorbax Eclipse XDB-C18, 4.6 × 150 mm, 5 μm particle size column with the flow rate 1 mL min-1, column temperature set at 30 °C and UV detection at 256 nm. The established method was then subjected to method validation and the required validation parameters were tested. For the robustness evaluation, fractional factorial 24-1 design was utilized and factors that might significantly affect the system performance were defined. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of itraconazole, its impurities B and F in any laboratory under different circumstances has been proven.

Development and Validation of a Reversed-Phase HPLC Method for Determination of Alkaloids from Papaver somniferum L. (Papaveraceae)

2012 ◽  
Vol 95 (2) ◽  
pp. 399-405 ◽  
Author(s):  
Jelena Acevska ◽  
Aneta Dimitrovska ◽  
Gjoshe Stefkov ◽  
Katerina Brezovska ◽  
Marija Karapandzova ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Reversed Phase ◽  
Hplc Method ◽  
Papaver Somniferum ◽  
Chromatographic Behavior ◽  
Organic Modifier ◽  
Column Temperature ◽  
Development And Validation

Abstract An HPLC method for the separation of six target alkaloids from Papaver somniferum L. (morphine, codeine, oripavine, thebaine, papaverine, and noscapine) was developed, optimized, and validated. The chromatographic behavior of these alkaloids was investigated using a reversed-phase chromatography at acidic and alkaline pH. The effects of ion-pairing agents, pH value of the mobile phase, concentration of the buffer components, mobile phase organic modifier, and column temperature were studied. Regardless of the large differences in their pKa values, all alkaloids were separated within a close retention window, and good peak shape was achieved for each of the six alkaloids. The proposed method has adequate selectivity, linearity, accuracy, precision, and reproducibility and is applicable for poppy straw.

scholarly journals Experimental design approach for the development and validation of an enantiospecific RP-HPLC method for simultaneous determination of clopidogrel and related compounds

2008 ◽  
Vol 27 (1) ◽  
pp. 53 ◽  
Author(s):  
Rumenka Petkovska ◽  
Claus Cornett ◽  
Aneta Dimitrovska
Keyword(s):  
Experimental Design ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Hplc Method ◽  
System Response ◽  
Buffer Solution ◽  
Column Temperature ◽  
Rp Hplc ◽  
Related Compounds

An enantiospecific RP-HPLC method was developed and validated for the simultaneous determination of clopidogrel and four related compounds specified as impurities. Experimental design was applied during the method optimization (Full factorial 23 design) and robustness testing (Central Composite Face Centered design). Laboratory mixtures of clopidogrel and its impurities in a concentration ratio of 1: 5.0×10–4 were used as an investigation matrix. The three independent variables were the acetonitrile content in the mobile phase, pH of the mobile phase, and the column temperature. A Chromatographic Response Function (CRF) was used for estimation of the system response resolution (Rs). Separation was achieved using mobile phase composition of ACN: Buffer solution pH 6.5 (40:60 v/v) at 30 ºC. A CHIRAL-AGP 4.0 mm × 100 mm, 5.0 μm particle size column was used. The total time for chromatographic separation was approximately 10.0 min. The method was validated for its selectivity, linearity, precision, accuracy and robustness.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

2021 ◽  
pp. 138-150
Author(s):  
Sachin B. Gholve ◽  
Jaiprakash N. Sangshetti ◽  
Omprakash G. Bhusnure ◽  
Ram S. Sakhare ◽  
Pratap H. Bhosale ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Drug Substance ◽  
Gastric Ulcers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

scholarly journals Determination of Ketotifen Fumarate in Syrup Dosage Form by High Performance Liquid Chromatography

2020 ◽  
pp. 63-72
Author(s):  
Mohammed Ali Salih ◽  
Dlivan Fattah Aziz ◽  
Salar Ibrahim Ali
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Ketotifen Fumarate ◽  
Suggested Technique ◽  
Elution Method

The goal of the current study was to establish and authenticate an isocratic reverse-stage High-Performance Liquid Chromatography (HPLC) method for quantifying ketotifen fumarate (KF) in pharmaceutical liquid dosage compositions. Easy, quick, accurate, exact, and accurate reverse-stage high-performance liquid chromatography was advanced for the simultaneous assessment of ketotifen fumarate in the liquid syrup dosage type. The HPLC system using isocratic elution method with reverse-phase Inertsil ODS-(250 mm × 4.6 mm, 3 μm) column was detected by ultraviolet absorbance at 297 nm with no interference from widely using excipients, the mobile phase (A) is a mixture of triethylamine and water (175 μl in 500 ml of water), and the mobile phase (B) is a mixture of triethylamine and methanol (175 μl in 500 ml of methanol) at a flow rate of 1.5 mL/min (mobile phase A 40 %:mobile phase B 60%) at column temperature using 40 ° C, the retention time for ketotifen fumarate was 6.4±0.5 min. The concentration curves were linear in the range of 10.0 to 35.0 μg / ml (R2 = 0.9999). The developed method was tested for the specificity, precision, linearity, precision, reliability, robustness, and consistency of the solution. The regeneration of ketotifen fumarate in formulations was found to be 99.75 %, 99.91 %, and 100.05 % respectively. The percent RSD for percent recovery was found to be 0.21 and 0.17 and 0.10 for ketotifen fumarate. In the conclusion, the suggested technique was successfully used for the quantitative determination of ketotifen fumarate in formulations.

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