scholarly journals Cost Effective, Efficient and Stability indicating analytical method validation for Ranolazine related by Reverse Phase High Performance Liquid Chromatography in drug substances

2020 ◽  
Vol 10 (6-s) ◽  
pp. 45-54
Author(s):  
Pushpendra Sharma ◽  
KLV Satyanarayana ◽  
G. Sri Hari
Keyword(s):  
Method Validation ◽  
Mobile Phase ◽  
High Performance ◽  
Cost Effective ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature ◽  
Analytical Method Validation ◽  
Drug Substances ◽  
Ich Guidelines

A simple, selective, linear, precise and accurate RP-HPLC method was developed and validated for rapid assay of Ranolazine in drug substances. Isocratic elution at a flow rate of 1.4ml/min was employed on Hypersil BDS C18, 150 x 4.6 mm, 5µm or Equivalent at 40°C column temperature. The mobile phase consisted of Mobile phase-A: Mobile phase-B (55:45) (Disodium hydrogen orthophosphate buffer with pH 7.0 and Acetonitrile). The UV detection wavelength was at 205 nm. Linearity was observed in concentration range of 0.07-0.82 ppm for ranolazine impurity-I and concentration range of 0.07-0.78 ppm for ranolazine impurity-II. The retention time for Ranolazine was 7.6 min. The method was validated for validation parameter like specificity, force degradation, linearity, accuracy, precision and robustness as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Ranolazine in pharmaceutical dosage forms. Keywords: Ranolazine, Method Validation, Drug Substances, HPLC

scholarly journals HPLC method validation for quantification of tetrahydrocurcumin in bulk drug and formulation

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Roopam Raut ◽  
Jessy Shaji
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Wide Spectrum ◽  
Cost Effective ◽  
Hplc Method ◽  
Uv Detector ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Recovery Study ◽  
Bulk Drug

Abstract Background Tetrahydrocurcumin (THC), the active metabolite of curcumin, is gaining popularity amongst scientist due to its wide spectrum of pharmacological activities, better stability and colourless nature. The objective of this study was to develop a sensitive, cost-effective RP-HPLC method for the estimation of THC in bulk drug substance and formulation. Results Efficient chromatographic separation was achieved on Hypersil BDS, C18 column, 250 mm × 4.6 mm, 5 μm column by isocratic elution with mobile phase comprising of acetonitrile: methanol: water (40:23:37% V/V); adjusted to a pH of 3.0 ± 0.05. The flow rate of the mobile phase was 1.0 ml/min with a column temperature of 25 °C. UV detector was used for the analysis and detection was carried out at 280 nm. The developed method was validated according to ICH guidelines with respect to system suitability, linearity, accuracy, precision and robustness. The theoretical plates were found to be more than 5800. The method showed linearity over the range of 4 to 60 μg/ml with R2 = 0.9998. The accuracy of the method in terms of recovery study was 98.23-99.99%. The %RSD for intra-day and inter-day precision were 0.272 and 0.275, respectively. The method was found to be robust with respect to change in wavelength, flow rate and column temperature. Conclusion The analytical method was found satisfactory on validation as per ICH guidelines. Hence, it can be routinely used for quantification of THC in bulk drug and formulation.

RP-HPLC METHOD FOR ESTIMATION OF LORNOXICAM IN TABLETS AND IN DISSOLUTION SAMPLES USING MASS SPECTROMETRIC COMPATIBLE BUFFERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Mass Spectrometric ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.

scholarly journals A Fast and Validated HPLC Method for Simultaneous Determination of Dopamine, Dobutamine, Phentolamine, Furosemide, and Aminophylline in Infusion Samples and Injection Formulations

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Fuchao Chen ◽  
Baoxia Fang ◽  
Sicen Wang
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Precision Data ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
The Stability

A simple, fast, and validated HPLC method was developed for the simultaneous quantization of five cardiovascular agents: dopamine (DPM), dobutamine (DBM), phentolamine (PTM), furosemide (FSM), and aminophylline (APL) either in infusion samples or in an injection dosage form. The proposed method was achieved with a 150 mm × 4.6 mm, 5.0 μm C18 column, by using a simple linear gradient. Mobile phase A was buffer (50 mM KH2PO4) and mobile Phase B was acetonitrile at a flow rate of 1.0 mL/min. The column temperature was kept at 30°C, and the injection volume was 20 μL. All analytes were separated simultaneously at a retention time (tr) of 3.93, 5.84, 7.06, 8.76, and 9.67 min for DPM, DBM, PTM, FSM, and APL, respectively, with a total run time of less than 15.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 12.0–240.0, 12.0–240.0, 20.0–200.0, 6.0–240.0, and 10.0–200.0 μg/mL DPM, DBM, PTM, FSM, and APL, respectively. Interday and intraday accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all five drugs in their injection dosage form, infusion samples, and for evaluation of the stability of investigated drugs in mixtures for endovenous use. The results of the stability study showed that mixtures of DPM, DBM, PTM, FSM, and APL in 5% glucose or 0.9% sodium chloride injection were stable for 48 hours when stored in polypropylene syringes at 25°C.

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 Simple, Accurate and Efficient High Performance Liquid Chromatographic Method for Determination of Vandetanib in Bulk and in Pharmaceutical Forms

2021 ◽  
pp. 153-160
Author(s):  
M. Murali ◽  
P. Venkateswara Rao
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, linear, precise and accurate isocratic RP-HPLC method was developed and validated for rapid assay of Vandetanib, an anticancer drug, in both bulk and tablet dosage form. Elution at a flow rate of 1ml/min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of acetonitrile, water and orthophosphoric acid in the ratio of 90:08:02 (v/v/v). Linearity was observed in concentration range of 50-200 ppm. The retention time for Vandetanib was 3.326 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Vandetanib in pharmaceutical dosage forms. Moreover the detection alone was also verified through LC-MS of the Vandetanib drug using ESI method which provides future scope for study of this drug using LC-MS method also.

scholarly journals Comparative Study on Quantification of Total Catechins Using UV-Vis Spectrophotometric Method and High Performance Liquid Chromatography Techniques

2021 ◽  
Vol 37 (1) ◽  
pp. 136-142
Author(s):  
Sitharanjan Kalidass ◽  
Karuppannau Daiyarvijaya ◽  
Rajagopal Raj Kumar
Keyword(s):  
Quantitative Analysis ◽  
Spectrophotometric Method ◽  
Mobile Phase ◽  
High Performance ◽  
Cost Effective ◽  
Hplc Method ◽  
Good Resolution ◽  
Huge Number ◽  
Automated Hplc

Bioavailability of catechinsin wider range of plants was established earlier and it’s utility as medicine against cardiovascular disease, cancer, etc. were also demonstrated. Recent techniques in relation to quantitative analysis of total catechins seem to be laborious and time consuming process to handle huge number of samples. Established spectrophotometry and HPLC methods developed earlier for quantitative determination of total catechins in tea extracts were compared in the present study.UV-Vis spectrophotometric method was adopted to monitor the absorbance at 500 nm of the reaction mixture (catechins and vanillin-H2SO4reagents). Hewlett Packard automated HPLC was used and equipped with Phenomenex Luna 5  phenyl-hexyl column fitted with a Phenomenex guard column. Binary elution was carried out using Mobile phase A (acetic acid and acetonitrile) and Mobile phase B (acetonitrile). Method adopted showed a good resolution of catechin fractions and was found to be accurate for the quantification of total catechins (sum of individual catechins). Results of the both the methods are comparable and variation amongst the two methods ranged between -3.59 and 2.79% among the clones and varied with seasons.As expected UPASI released tea clones exhibited variations in their bioavailability. Lean season edge over the cropping period sampling in terms of total catechins. Results obtained from both the methods are comparable. Two methods can be used for the routine quantitative analysis of total catechins; however, spectrophotometric method found to be simple, rapid and cost effective than that of HPLC method unless individual catechins composition is warranted.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

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.

Analysis of Bifenthrin and its Enantiomer Using High Performance Liquid Chromatography

2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Column Temperature ◽  
Polysaccharide Derivatives ◽  
Separation Results

Using the high performance liquid chromatography (HPLC) method, bifenthrin isomers can be split at a polysaccharide derivatives chiral stationary phase column, and two well distinguished peaks of bifenthrin isomers are obtained. The effects of mobile phase ratios, temperatures, and detection wavelengths on the separation results are discussed. The optimal chromatographic conditions are as follows: the mobile phase ratio is methanol: ammonium acetate salts = 80:20, the column temperature is 35°C, and the wavelength is set as 220 nm. Under the optimal conditions, the resolution of bifenthrin enantiomer can be as large as 3.0.

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