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 DEVELOPMENT AND VALIDATION OF RP-CHIRAL HPLC METHOD FOR QUANTIFICATION OF (S)-ISOMER IN TENOFOVIR DISOPROXIL FUMARATE

2017 ◽  
Vol 9 (6) ◽  
pp. 31
Author(s):  
Suresh Babu Bodempudi ◽  
Ravi Chandra Babu Rupakula ◽  
Konda S. Reddy
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
Mobile Phase ◽  
Linear Regression Analysis ◽  
Hplc Method ◽  
Drug Substance ◽  
Phase System ◽  
Chiral Hplc ◽  
Column Temperature ◽  
Relative Standard

Objective: The main objective of present study was to develop and validate a reverse phase enantioselective chiral high performance liquid chromatographic method was developed for enantiomeric resolution of Tenofovir disoproxil fumarate; it decreases the HIV infection in human body. The method is specific, rapid, precise and accurate for the separation and determination of (S)-isomer in tenofovir disoproxil fumarate drug substance form.Methods: The S-Isomer of Tenofovir disoproxil fumarate was resolved on a Chiral AGP (150 × 4.0 mm, 5 µm) column (L-41) using a mobile phase system containing 0.1 M ammonium acetate in water pH 6.8 with ammonia solution and methanol in the ratio of (85:15 v/v). The mobile phase was set at a flow rate of 0.8 ml/min and the volume injected was 10μl for every injection. The detection wavelength was set at 260 nm and the column temperature was set at 15 °C.Results: The proposed method was productively applied for the quantitative determination of (S)-isomer in Tenofovir disoproxil fumarate drug substance form. The linear regression analysis data for calibration plots showed a good linear relationship over a concentration range of 0.125 to 3.75 µg/ml for (S)-isomer, 0.125-3.75 µg/ml for Tenofovir disoproxil fumarate. The mean values of the correlation coefficient were 0.999 and 0.999 for (S)-isomer and Tenofovir disoproxil fumarate. The method was validated as per the ICH guidelines. The detection limit (LOD) was about 0.05 µg/ml and quantitation limit (LOQ) was about 0.125 µg/ml for (S)-isomer and Tenofovir disoproxil fumarate. The relative standard deviation was found to be 0.78 % for (S)-isomer in Tenofovir disoproxil fumarate.Conclusion: The developed and validated HPLC method and the statistical analysis showed that the method is repeatable and selective for the estimation of the (S)-isomer of the Tenofovir disoproxil fumarate drug substance.

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 The identification and the quantitative determination of loratadine by the HPLC method

2021 ◽  
Vol 19 (3(75)) ◽  
pp. 40-46
Author(s):  
Olena O. Mamina ◽  
Volodymyr I. Kabachny ◽  
Nataliia Yu. Bondarenko ◽  
Olena V. Lozova
Keyword(s):  
Quantitative Determination ◽  
Mobile Phase ◽  
Hplc Analysis ◽  
Hplc Method ◽  
Therapeutic Monitoring ◽  
Reproducible Research ◽  
Column Temperature ◽  
Model Solutions ◽  
Relative Standard

Aim. To develop the unified method of the HPLC analysis of loratadine, which can allow obtaining reliable and reproducible results of the studies of pharmaceuticals and biological matrices for monitoring the treatment effectiveness.Materials and methods. The HPLC analysis was performed on a “Milichrome A-02” microcolumn liquid chromatograph under the following conditions: a reversed-phase variant, 2 × 75 mm column filled with a non-polar sorbent Prontosil 120-5 C18 AQ, 5 μm; the mobile phase in the mode of a linear gradient – from eluent А (5 % of acetonitrile and 95  % of a buffer solution) to eluent B (100 % of acetonitrile) for 40 min. The flow rate of the mobile phase was 100 μL/min; the injection volume was 4 μL. The multichannel detection of the substance was carried out using an UV-detector at 210, 220, 230, 240, 250, 260, 280 and 300 nm; the optimal value of the column temperature was 37 – 40 °С, and the pump pressure was 2.8 – 3.2 MPa.Results and discussion. As a result of the studies performed, the retention parameters of loratadine and spectral relationships were determined using the unified HPLC method. This made it possible to include the results obtained in the database for the identification of antihistamines in the therapeutic monitoring of the treatment with an individual drug or in the complex treatment of allergic reactions. The development of the quantitative determination of loratadine by HPLC on model solutions using various concentrations of the drug was carried out. The content of loratadine was determined by the equation S = 1.14 × 10-3C – 0.50 × 10-4; the correlation coefficient was 0.9998. It was found that the relative standard deviation RSD did not exceed 0.93 % when analyzing loratadine in the model solutions by HPLC.Conclusions. The identification and the quantitative determination of loratadine by the unified HPLC method have been conducted. The method allows obtaining reliable and reproducible research results. The results of the studies can be recommended for implementation in the practice of forensic bureaus, toxicological centers, and clinical laboratories.

RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF AMPHOTERICIN B

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
Author(s):  
L Mohankrishna ◽  
◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya
Keyword(s):  
Amphotericin B ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Phase Combination ◽  
Hplc Method Development

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

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 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 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.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

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.

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