scholarly journals Chemometrically assisted RP-HPLC method development for efficient separation of ivabradine and its eleven impurities

2020 ◽  
Vol 32 (1) ◽  
pp. 53-63 ◽  
Author(s):  
Jovana Tomić ◽  
Branka Ivković ◽  
Slavica Oljačić ◽  
Katarina Nikolić ◽  
Nevena Maljurić ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Chromatographic Retention ◽  
Positional Isomers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Efficient Separation ◽  
Rp Hplc

The aim of this study was to develop a novel reversed-phase high-performance liquid chromatography (RP-HPLC) method for efficient separation of ivabradine and its 11 impurities. Similar polarity of impurities in the sample mixture made method optimization challenging and accomplishable only when different chemometric tools, such as principal component analysis (PCA), Box–Behnken design (BBD), and desirability function as a multicriteria approach, were employed. The presence of 3 positional isomers (impurities III, V, and VI), keto–enol tautomerism of impurity VII, and diastereoisomers of impurity X made separation of this complex mixture even more challenging. Chromatographic retention parameters obtained with the mobile phase consisting of 30 mM phosphate buffer and acetonitrile (80:20, v/v) on four different RP-HPLC columns at varying pH values (3.0, 4.0, and 5.0) were subjected to the PCA analysis to select the column with the most appropriate selectivity. Then the column temperature, pH of the aqueous component of mobile phase, phosphate buffer molarity and the organic solvent content in the mobile phase were estimated employing BBD. Valid and reliable mathematical models towards resolution of twelve critical peak pairs were obtained. After determination of the desirability making criteria for all responses, desirability functions were established and used in optimization. The proposed optimal chromatographic conditions included the Zorbax Eclipse Plus C18 chromatographic column (100 × 4.6 mm, 3.5 μm), the column temperature of 34 °C, the mobile phase flow rate of 1.6 mL min−1 and the UV detection at 220 nm. The mobile phase consisted of the 28 mM phosphate buffer at pH 6.0 and acetonitrile (85:15, v/v). Separation of one pair of positional isomers was not achieved, so methanol was added to the organic part of mobile phase in small increments with the optimal ratio of methanol to acetonitrile 59:41, v/v. The overall organic component of the mobile phase also increased to 18%, accelerating the chromatographic analysis.

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.

Method Development and Validation of Degradation Studies of Lenalidomide by RP-HPLC

2021 ◽  
pp. 4281-4286
Author(s):  
Punna Venkateshwarlu ◽  
Mehul M. Patel
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
System Suitability ◽  
Wide Range

A simple, accurate, RP HPLC method was developed by this study determination of lenalidomide. This method is developed by Shimadzu LC -2010 HT by using C18 (250 X 4.6 X mm X 5µ) column in solvents Phosphate buffer: Acetonitrile (55:45) v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate 1ml/min was pumped and sample wavelength was detected at 242nm by ultraviolet -visible spectrophotometer. The retention time was found 2.5 min. The number of theoretical plates and tailing factor for lenalidomide was observed 16199.817 (NLT 2000) and 1.128 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, system suitability and robustness. LOD and LOQ values obtained from regression of lenalidomide 0.058 and 0.174µg/ml. The regression equation of validated method for lenalidomide is Y=5223x+183075. In wide range of 25 to 150 (µg/ml) the linearity was observed. The method was validated and a recovery study indicates accuracy of this method. The Retention time less compared to established methods. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lenalidomide in bulk drug and in its pharmaceutical dosage forms.

scholarly journals Method Development and Validation of Fludrocortisone Acetate Tablets by Reverse Phase HPLC Method

2020 ◽  
Vol 11 (4) ◽  
pp. 6826-6833
Author(s):  
Vijey Aanandhi M ◽  
Elancheziyan K ◽  
Yamini R ◽  
Prakash Chand T ◽  
Aysha Jadeera K A ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Hplc Technique ◽  
Fludrocortisone Acetate ◽  
Development And Validation

The purpose or intent of this current study was to establish a fast and sensitive HPLC technique for the perseverance of Fludrocortisone acetate and utilizing best frequently used HPLC technique. This method had been validated as per the ICH requirements  to assure that the method consistently meets the predetermined specifications and quality attributes.Utilizing filtered and degassed pH 3.0 Phosphate buffer and Acetonitrile in the ratio 90:10 as a Mobile phase-A and pH 3.0 Phosphate buffer and Acetonitrile in the ratio 65:35 as a Mobile phase-B the established RP-HPLC technique was done. The separation was achieved by using Waters, X-Bridge Shield RP18, (150 X 4.6-mm), 3.5-µm column. Run time and Flow rate was set 45minutes and 1.2mL/min. Injection volume 100µL and wavelength was set 240nm.The correlation coefficient square for fludrocortisones acetate and Fludrocortisone Impurity was found to be 0.9991 and 0.99997. The SD and %RSD for Fludrocortisone Impurity was found to be 0.02 and 1.48 represents method precision. Following validated parameters lies within the limit. Hence, the developed method was precise, simple, fast and accurate.

Method Development and Validation for Estimation of related Substances in Tilorone Dihydrochloride using RP¬-HPLC

2021 ◽  
pp. 3319-3324
Author(s):  
M. Zeba Baktiyar ◽  
B. Mohammed Ishaq ◽  
Siva Sanker Reddy L ◽  
Sreenivasulu M.
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Column Temperature ◽  
Related Substances ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and reproducible RP-HPLC method was developed for the estimation of related substances in tilorone dihydrochloride. Quantification was performed using a Zorbax SB-phenyl column (150 × 4.6mm, 5µ) with mobile phase A: 20mM potassium dihydro phosphate + 2ml of triethylamine, pH 2.30 and mobile phase B: acetonitrile, methanol and water 60: 20: 20% v/v. A gradient program was followed with a run time of 55 minutes at a flow rate of 1.0 ml/min. The column temperature was maintained at 40°C, the injection volume was 10 µl and the detection was performed at 269nm using a PDA detector. The retention time of Tilorone dihydrochloride was found to be 10.36 minutes. The proposed method has been validated according to the ICH guidelines for Linearity, Precision, Accuracy, LOD, and LOQ. The method was linear from 0.157 - 3.934μg/ml for standard, 0.153-3.820μg/ml and 0.166 - 4.140μg/ml for impurities, TLHC01 and TLHC02 respectively. The impurities TLHC01 and TLHC02 have been mapped in all stress conditions. The LOD and LOQ of TLHC01 were found at 1.757μg/ml and 5.857μg/ml and 1.919μg/ml and 6.396μg/ml respectively for TLHC02 respectively. Statistical analysis showed that the method was precision, reproducible, selective, specific and accurate for the analysis of Tilorone dihydrochloride and its impurities. The wide range of linearity, sensitivity, precision, short retention times and simple mobile phase have shown that the method is suitable for the routine quantification of mass impurities of tilorone hydrochloride and its dosage pharmaceutical forms with high precision and accuracy.

scholarly journals Method Development and Validation of Degradation Studies of Favipiravir by RP-HPLC

2021 ◽  
pp. 220-228
Author(s):  
. Shyamala ◽  
Dongamanti Ashok
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Analytical Standards ◽  
Theoretical Plates

RP HPLC method was developed by this study estimation of favipiravir. This method is developed by Shimadzu LC -2010 HT by using a C18 (250 X 4.6 X mm X 5µ) column in solvents Water(OPA)+ACN  (60:40)v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate of 1ml/min was pumped and sample wavelength was detected at 324 nm by ultraviolet -visible spectrophotometer. The Rt was found 4.453 min. The number of theoretical plates and tailing factor for favipiravir was observed 82651(NLT 2000) and 1.265 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, LOD, LOQ and robustness. LOD and LOQ values were calculated from regression of favipiravir 1.26 and 3.83 µg/ml.The regression equation of validated method for favipiravir is Y=253.5x+1881.In a wide range of 4 to 20 (µg/ml) the linearity was observed. Degradation methods were also performed.

NEW VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF RIZATRIPTAN BENZOATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (12) ◽  
pp. 32-36
Author(s):  
T. Vishalakhi ◽  
◽  
S. K Kumar ◽  
K Sujana ◽  
P Rani
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Detector Response ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Rp Hplc ◽  
Bulk Drug

A simple validated RP HPLC method for the estimation of rizatriptan benzoate in pharmaceutical dosage form and bulk was developed for routine analysis. This method was developed by selecting Agilent TC C18 (250 x 4.6 mm, 5 μ) column as stationary phase and acrylonibrile:water (45:55), pH adjusted to 3, as mobile phase. Flow rate of mobile phase was maintained at 4: 1 mL/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 220 nm. The retention time obtained for rizatriptan was 2.8 min. The detector response was linear in the concentration range of 2-25μg/mL. This method was validated and shown to be specific, sensitive, precise, linear, accurate, rugged and robust. Hence, this method can be applied for routine quality control of rizatriptan benzoate in dosage forms as well as in bulk drug.

scholarly journals RP-HPLC Method Development and Its Validation for Quantitative Determination of Rimonabant in Human Plasma

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Shravan Bankey ◽  
Ganesh Tapadiya ◽  
Jasvant Lamale ◽  
Deepti Jain ◽  
Shweta Saboo ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Hplc Method Development

A simple, accurate, and precise HPLC method was developed and validated for determination of rimonabant in human plasma. Following liquid-liquid extraction, chromatographic separation was accomplished using C18 column with mobile phase consisting of acetonitrile : water (90 : 10, v/v), drug was detected at 260 nm using UVdetector. The LOD and LOQ were 3.0 and 10.0 μg/L, respectively. The method is linear in the interval 50.0–1000.0 μg/L. The average extraction recovery of drug from plasma was found to be 92.2%. The percent CV of the method was found to be less than 10.8%, and accuracy was found between 94.5 and 106.7%. The assay may be applied to a pharmacokinetic and bioequivalence study of rimonabant.

scholarly journals Method Development and Validation of RP-HPLC Method for the Estimation of Ormeloxifene

2017 ◽  
Vol 2 (03) ◽  
pp. 78-82
Author(s):  
Anusha Shivaraj ◽  
Shireesha Battula
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Isocratic Mode ◽  
Ich Guideline

A new simple, specific, accurate, precise RP-HPLC method has been developed for the estimation of Ormeloxifene. The chromatographic separation for Ormeloxifene was achieved with mobile phase containing methanol :ACN(70:30 v/v), agilent C18 column (4.6 x150 mm) 5 μ at room temperature and UV detection at 274nm.The compounds were eluted in the isocratic mode at a flow rate of 1ml/min. The retention time of Ormeloxifene was found to be 2.497min. The method was validated according to ICH guideline for linearity, specificity, precision, accuracy, LOD, LOQ and robustness in accordance with ICH guidelines.

RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF LINAGLIPTIN AND EMPAGLIFLOZIN

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (05) ◽  
pp. 68-71
Author(s):  
A Lakshmana Rao ◽  
◽  
T. Prasanthi ◽  
E. L Anusha
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

A simple, accurate and precise RP-HPLC method was developed for the simultaneous estimation of the linagliptin and empagliflozin in tablet dosage form. Chromatogram was run through Kromasil 250 x 4.6 mM, 5mM column, mobile phase containing 0.1% o-phosphoric acid buffer and acetonitrile in the ratio of 60:40%v/v was pumped through column at a flow rate of 1 mL/min. The optimized wavelength was 230 nm. Retention times of linagliptin and empagliflozin were found to be 2.759 min and 2.139 min. %RSD of the Linagliptin and Empagliflozin were found to be 0.5 and 0.6 respectively. Percentage assay was obtained as 99.91% and 100.15% for linagliptin and empagliflozin, respectively. LOD, LOQ values obtained for linagliptin and empagliflozin were 0.23 μg/ml and 0.44 μg/mL and 0.70 μg/mL and 1.34 μg/mL, respectively. Thus, the current study showed that the developed RP-HPLC method is sensitive and selective for the estimation of linagliptin and empagliflozin in combined dosage form.

RP-HPLC METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (10) ◽  
pp. 68-70
Author(s):  
K. Sankar ◽  
◽  
A. P. Jadhav
Keyword(s):  
Immune Response ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Rp Hplc ◽  
Marker Compounds ◽  
Hplc Method Development

Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively, were used as marker compounds for developing a simple, accurate, precise and robust RP-HPLC method for simultaneous estimation from Talekt capsule. It is a polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. The mobile phase of methanol: 1% ortho phosphoric acid in water in the ratio of 90:10 V/V was used for separation. Retention time of curcumin and embelin were found to be 2.77 ± 0.2 minutes and 7.77 ± 0.2 minutes, respectively. The developed method was validated as per ICH Q2 (R1) guidelines.

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