scholarly journals Improved Achiral and Chiral HPLC-UV Analysis of Ruxolitinib in Two Different Drug Formulations

Separations ◽  
2020 ◽  
Vol 7 (3) ◽  
pp. 47
Author(s):  
Alessandro Di Michele ◽  
Aurélie Schoubben ◽  
Ina Varfaj ◽  
Alessandro D’Arpino ◽  
Laura Mercolini ◽  
...  
Keyword(s):  
Stationary Phases ◽  
Retention Factor ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Enantiomeric Purity ◽  
Chiral Hplc ◽  
Drug Formulations ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability

In this paper, two new reversed-phase (RP) HPLC-UV methods enabling the quantitative achiral and chiral analysis of ruxolitinib in commercial tablets (containing 20 mg of active pharmaceutical ingredient, API) and not commercially available galenic capsules (with 5 mg of API) are described. For the achiral method based on the use of a water/acetonitrile [70:30, v/v; with 0.1% (v) formic acid] eluent, a “research validation” study was performed mostly following the “International Council for Harmonization” guidelines. All the system suitability parameters were within the acceptance criteria: tailing factor, between 1.7 and 2.0; retention factor, 2.2; number of theoretical plates, >9000. The linearity curve showed R2 = 0.99 (Rxv2 = 0.99), while trueness (expressed as recovery) was between 96.3 and 106.3%. Coefficient of variations (CVs) (repeatability: CVw and intermediate precision: CVIP) did not exceed 1.3% and 2.9%, respectively. Moreover, the use of the enantiomeric Whelk-O1 chiral stationary phases operated under similar RP eluent conditions as for the achiral analyses, and the “inverted chirality columns approach (ICCA)” allowed us to establish that the enantiomeric purity of ruxolitinib is retained upon reformulation from tablets to capsules. The two developed methods can allow accurate determinations of ruxolitinib in drug formulations for medical use.

scholarly journals Reversed-Phase HPLC Analysis of Levetiracetam in Tablets Using Monolithic and Conventional C18 Silica Columns

2010 ◽  
Vol 93 (4) ◽  
pp. 1077-1085 ◽  
Author(s):  
Nafiz O Can ◽  
Goksel Arli
Keyword(s):  
Monolithic Column ◽  
Stationary Phases ◽  
Internal Standard ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Tablets ◽  
System Suitability ◽  
Development And Validation

Abstract Development and validation of an RP-HPLC method for determination of levetiracetam in pharmaceutical tablets is described. The separation and quantification of levetiracetam and caffeine (internal standard) were performed using a single analytical procedure with two different types of stationary phases, conventional Phenomenex Gemini C18 (100 4.6 mm, 5 m) and Merck Chromolith Performance RP18e (100 4.6 mm, macropore size 2 mm, micropore size 13 nm) monolithic silica. Five-microliter aliquots of samples were injected into the system and eluted using wateracetonitrile (90 + 10, v/v) mobile phase pumped at the rate of 1 mL/min. The analyte peaks were detected at 200 nm using a diode array detector with adequate resolution. Validation studies were performed using the method recommended by the International Conference on Harmonization, the U.S. Pharmacopeia, and AOAC INTERNATIONAL, which includes accuracy, precision, range, limits, robustness, and system suitability parameters. Levetiracetam and caffeine were detected in about 7 min using the conventional column, whereas less than 5 min was required when the monolithic column was used. Calibration plots had r values close to unity in the range of 0.88.0 g/mL. Assay of levetiracetam in a tablet formulation was demonstrated as an application to real samples.

Chiral Chromatography Studies of Chemical Behavior of Cinacalcet on Polysaccharide Chiral Reversed-Phase HPLC Stationary Phases

2012 ◽  
Vol 95 (6) ◽  
pp. 1639-1643 ◽  
Author(s):  
Michal Douša ◽  
Jiřiacute; Břicháč
Keyword(s):  
Chiral Stationary Phase ◽  
Stationary Phases ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Chiral Chromatography ◽  
Chemical Behavior ◽  
Analytical Resolution

Abstract A rapid HPLC method for the analytical resolution of cinacalcet enantiomers was developed. Four chiral columns (two amylose and two cellulose type) were evaluated in RP systems. Excellent enantioseparation with a resolution of more than 6 was achieved on Chiralpak AY (amylose 5-chloro-2-methylphenylcarbamate chiral stationary phase) using 10 mM triethylamine (pH 8.0)–acetonitrile (40 + 60, v/v) mobile phase. Validation of the HPLC method, including linearity, LOD, LOQ, precision, accuracy, and selectivity, was performed according to the International Conference on Harmonization guidelines. The method was successfully applied for the determination of (S)-cinacalcet in enantiopure active pharmaceutical ingredient (R)-cinacalcet.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Hydroxylamine Hydrochloride content) in Leflunomide by using RP-HPLC technique

2021 ◽  
Vol 37 (02) ◽  
pp. 493-498
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hydroxylamine Hydrochloride ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective, linear having accuracy and specific of reverse phase high-performance liquid chromatographic (RP-HPLC) method for determination of Genotoxic impurity Hydroxylamine Hydrochloride of drug Leflunomide is reported.The separation and analysis were done on YMC Triart C18 (4.6 mm x 150 mm), having particle size 3.0 μm. KH2PO4 in 2000 mL of purified water and 2 mL triethylamine with pH 2.5 with phosphoric acid is mobile phase-A while acetonitrile is mobile Phase-B with gradient program. The elution achieved with 1.50 mL/min flow rate and using UV detection at 230 nm wavelength. Selected column oven temperature is 45°C and auto sampler 5°C respectively. In this method linearity and accuracy of Hydroxylamine HCl covered with specification limit of LOQ to 150 % (i.e.3 to 23 ppm). The observed correlation coefficient is 0.99965 and recovery in between 99.07 to 114.94. In method precision (ie.repeatability) and intermediate precision (IP) observed % RSD of six spiked test preparation is below 5.0 %. The standard and sample were stable for 3 days when stored at 2 to 8°C temperature. In robustness studies system suitability parameters ie tailing factor, theoretical plates and %RSD does not show significant changes. The present RP-HPLC method is selective, robust, linear, and precise for detection of Hydroxylamine HCl.

scholarly journals In vitro Dissolution Profile at Different Biological pH Conditions of Hydroxychloroquine Sulfate Tablets Is Available for the Treatment of COVID-19

2021 ◽  
Vol 7 ◽  
Author(s):  
Thirupathi Dongala ◽  
Naresh Kumar Katari ◽  
Santhosh Kumar Ettaboina ◽  
Anand Krishnan ◽  
Murtaza M. Tambuwala ◽  
...  
Keyword(s):  
Antimalarial Activity ◽  
Reversed Phase ◽  
In Vitro Dissolution ◽  
Dissolution Profile ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Relative Standard ◽  
Ph Conditions ◽  
Clinical Experiments

Hydroxychloroquine sulfate is one of an extensive series of 4-aminoquinolines with antimalarial activity. Moreover, it is used for the treatment of rheumatoid arthritis. Sometimes, hydroxychloroquine sulfate is beneficial for the treatment of autoimmune diseases. Based on recent clinical experiments, it is exploited for the treatment of COVID-19, coronavirus across the globe. The chromatogram separation was achieved by using Agilent, Zorbax C8, 250 mm × 4.6 mm i.d., column. The buffer consists of 0.01 M of 1-pentane sulfonic acid and 0.02% of orthophosphoric acid in purified water. Mixed buffer, acetonitrile, and methanol (800:100:100 v/v). The flow rate was 1.0 ml min−1, and injection volume was 10 μl. Detection was made at 254 nm by using a dual absorbance detector (DAD). The reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated as per the current International Conference on Harmonization (ICH) guidelines to estimate hydroxychloroquine sulfate tablets. As part of method validation, specificity, linearity, precision, and recovery parameters were verified. The concentration and area relationships were linear (R2 > 0.999) over the concentration range of 25–300 μg ml−1 for hydroxychloroquine (HCQ). The relative standard deviations for precision and intermediate precision were <1.5%. The proposed RP-HPLC generic method was applied successfully to evaluate the in vitro dissolution profile with different pH conditions such as 0.1 N HCl, pH 4.5 acetate buffer, and pH 6.8 phosphate buffers as US-marketed reference products.

scholarly journals A Validated RP HPLC-PAD Method for the Determination of Hederacoside C in Ivy-Thyme Cough Syrup

2010 ◽  
Vol 2010 ◽  
pp. 1-5 ◽  
Author(s):  
Ayman Khdair ◽  
Mohammad K. Mohammad ◽  
Khaled Tawaha ◽  
Eman Al-Hamarsheh ◽  
Hatim S. AlKhatib ◽  
...  
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Phase System ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Cough Syrup

A simple reversed phase high-performance liquid chromatographic (RP-HPLC) method coupled with a photodiode array detector (PAD) has been developed and validated for the analysis of hederacoside C, the marker of ivy plant, in Ivy-Thyme cough syrup. Separation of hederacoside C was achieved using a Phenomenex-Gemini C18 column isothermally at C. A mobile phase system constituted of solvent A (water: acetonitrile: orthophosphoric acid (85%), 860 : 140 : 2 v/v) and solvent B (acetonitrile: orthophosphoric acid (85%), 998 : 2 v/v) was used, at gradient conditions, at a flow rate of 1.5 mL/min. Analysis was performed using UV-detection (205 nm). The method was linear over the range (0.03–0.15) mg/mL of hederacoside C (). Repeatability and intermediate precision were acceptable (RSD %). Limits of detection (LOD) and quantitation (LOQ) were 0.011 and 0.032 mg/mL, respectively. Percentage recovery was found to lie between 99.69% and 100.90% (RSD %). The method was also proved to be specific (peak-purity ).

scholarly journals ANALYTICAL QUALITY-BY-DESIGN (AQBD) APPROACH FOR THE DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF LAMOTRIGINE IN BULK AND TABLET FORMULATION

2021 ◽  
Vol 10 (5) ◽  
pp. 3591-3596
Author(s):  
Manisha P. Puranik
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Ich Guideline

The current analytical exploration illustrated developing a reversed-phase high-performance liquid chromatography (RP-HPLC) technique and consequent substantiation for analyzing lamotrigine (LAM) active pharmaceutical ingredient (API) using a Quality-by-design (QbD) approach (Central Composite Design), in bulk product as well as in the tablet formulations. In this experiment, based on systematic scouting, four key components (viz., mobile phase, column, flow-rate, and wavelength) were studied by the RP-HPLC method. 13 experimental runs were done with acetonitrile (ACN) (40-60% v/v) having flow-rate in the range 0.8 mL/min to 1.2 mL/min. The proposed analytical method was thoroughly corroborated in terms of ruggedness linearity, robustness, accuracy, and precision in accordance with ICH guideline Q2A and ICH guideline Q2B. Under the optimum chromatographic environment; Intersil C8 column of 250 mm length, 4.6 mm (i.d.); 20 μL injection volume; and mobile phase ACN: Methanol (60:40 v/v), a retention time of 2.542 min was noticed at 220 nm detection wavelength. The method was found to be extremely reproducible, accurate, linear, precise, robust, and economically adequate to execute the estimation. The intended analytical technique was thoroughly assessed through statistical tools and could be an imperative concern for the habitual scrutiny of LAM in bulk products and its formulation.

scholarly journals Retention Modelling of Phenoxy Acid Herbicides in Reversed-Phase HPLC under Gradient Elution

Molecules ◽  
2020 ◽  
Vol 25 (6) ◽  
pp. 1262 ◽  
Author(s):  
Alessandra Biancolillo ◽  
Maria Anna Maggi ◽  
Sebastian Bassi ◽  
Federico Marini ◽  
Angelo Antonio D’Archivio
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Retention Factor ◽  
Reversed Phase ◽  
Model Complexity ◽  
Retention Data ◽  
Rp Hplc ◽  
Phenoxy Acid Herbicides ◽  
Acid Herbicides ◽  
Phenoxy Acids

Phenoxy acid herbicides are used worldwide and are potential contaminants of drinking water. Reversed phase high-performance liquid chromatography (RP-HPLC) is commonly used to monitor phenoxy acid herbicides in water samples. RP-HPLC retention of phenoxy acids is affected by both mobile phase composition and pH, but the synergic effect of these two factors, which is also dependent on the structure and pKa of solutes, cannot be easily predicted. In this paper, to support the setup of RP-HPLC analysis of phenoxy acids under application of linear mobile phase gradients we modelled the simultaneous effect of the molecular structure and the elution conditions (pH, initial acetonitrile content in the eluent and gradient slope) on the retention of the solutes. In particular, the chromatographic conditions and the molecular descriptors collected on the analyzed compounds were used to estimate the retention factor k by Partial Least Squares (PLS) regression. Eventually, a variable selection approach, Genetic Algorithms, was used to reduce the model complexity and allow an easier interpretation. The PLS model calibrated on the retention data of 15 solutes and successively tested on three external analytes provided satisfying and reliable results.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Hydroxylamine Hydrochloride content) in Leflunomide by using RP-HPLC technique

2021 ◽  
Vol 37 (2) ◽  
pp. 493-498
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hydroxylamine Hydrochloride ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective, linear having accuracy and specific of reverse phase high-performance liquid chromatographic (RP-HPLC) method for determination of Genotoxic impurity Hydroxylamine Hydrochloride of drug Leflunomide is reported.The separation and analysis were done on YMC Triart C18 (4.6 mm x 150 mm), having particle size 3.0 μm. KH2PO4 in 2000 mL of purified water and 2 mL triethylamine with pH 2.5 with phosphoric acid is mobile phase-A while acetonitrile is mobile Phase-B with gradient program. The elution achieved with 1.50 mL/min flow rate and using UV detection at 230 nm wavelength. Selected column oven temperature is 45°C and auto sampler 5°C respectively. In this method linearity and accuracy of Hydroxylamine HCl covered with specification limit of LOQ to 150 % (i.e.3 to 23 ppm). The observed correlation coefficient is 0.99965 and recovery in between 99.07 to 114.94. In method precision (ie.repeatability) and intermediate precision (IP) observed % RSD of six spiked test preparation is below 5.0 %. The standard and sample were stable for 3 days when stored at 2 to 8°C temperature. In robustness studies system suitability parameters ie tailing factor, theoretical plates and %RSD does not show significant changes. The present RP-HPLC method is selective, robust, linear, and precise for detection of Hydroxylamine HCl.

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