scholarly journals Enantiomeric Separation of Colchicine and Lacosamide by Nano-LC. Quantitative Analysis in Pharmaceutical Formulations

Separations ◽  
2020 ◽  
Vol 7 (4) ◽  
pp. 55
Author(s):  
Natalia Casado ◽  
Zhengjin Jiang ◽  
María Ángeles García ◽  
María Luisa Marina
Keyword(s):  
Chiral Stationary Phase ◽  
Capillary Column ◽  
Pharmaceutical Formulations ◽  
Enantiomeric Separation ◽  
Chiral Drugs ◽  
Analytical Methodology ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Nano Liquid Chromatography

A chiral analytical methodology was developed by nano-liquid chromatography (nano-LC) enabling the enantiomeric separation of two chiral drugs, lacosamide (novel antiepileptic drug) and colchicine (antiuremic drug), commercialized as pure enantiomers. A capillary column lab-packed with an amylose tris(3,5-dimethylphenylcarbamate) chiral stationary phase was used in a lab-assembled nano-LC system. Lacosamide and colchicine enantiomers were separated in less than 8.0 and 9.0 min, respectively, with resolution values of 1.6 and 2.3, using 20 nL of sample and 1.8 µL of mobile phase per analysis. The analytical characteristics of the proposed methodology were evaluated according to the International Council for Harmonisation (ICH) guidelines, showing good analytical performance with good recoveries (97–98% and 100–103%) and precision values (relative standard deviation (RSD) <10.5 and <3.0%) for lacosamide and colchicine enantiomers, respectively. LODs were 1.7 and 2.0 µg/mL for (S)- and (R)-lacosamide, respectively, and 1.0 µg/mL for both colchicine enantiomers. Additionally, the developed methodology enabled to detect a 0.1% of the enantiomeric impurities, fulfilling the ICH regulation requirements. The method was applied to the determination of lacosamide and colchicine enantiomers in different pharmaceutical formulations to ensure their quality control. The content of the enantiomeric impurities was below a 0.1% and the amount of (R)-lacosamide and (S)-colchicine agreed with their labeled contents.

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, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals The simultaneous spectrophotometric determination of trimazolin and phenylephrine hydrochloride in nasal preparations

2008 ◽  
Vol 14 (4) ◽  
pp. 261-264 ◽  
Author(s):  
Ivana Savic ◽  
Goran Nikolic ◽  
Ivan Savic ◽  
Vladimir Bankovic
Keyword(s):  
Spectrophotometric Determination ◽  
Pharmaceutical Formulations ◽  
Active Components ◽  
Phenylephrine Hydrochloride ◽  
Drug Substances ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Relative Standard ◽  
High Degree

This paper presents the experimental results for the simultaneous spectrophotometric determination of two active components in nasal solutions. The resolution of two-component mixtures of timazolin and phenylephrine has been accomplished by using partial least-squares. The method comprised of the absorptivity measurement in a nasal solution at wavelengths of 265 and 272 nm, respectively. Notwithstanding the presence of two components and their high degree of spectral overlap, they have been determined simultaneously with high accuracy and precision, with no interference, rapidly and without resorting to extraction procedures using non aqueous solvents. This method was tested and validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2 %), while being simple, cheap and less time consuming. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

scholarly journals Development and validation of colorimetric method for the determination of pregabalin in bulk and pharmaceutical formulations

2020 ◽  
Vol 11 (4) ◽  
pp. 5896-5901
Author(s):  
Areej Abdelmonim Mohamed ◽  
Tilal Elsaman ◽  
Mohammed E Adam ◽  
Elrasheed A Gadkariem ◽  
Shaza W Shantier
Keyword(s):  
Colorimetric Method ◽  
Pharmaceutical Formulations ◽  
Colored Complex ◽  
Standardized Residuals ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Complex Development ◽  
Reaction Stoichiometry ◽  
Development And Validation

A simple, accurate and precise colorimetric method was developed for the quantification of pregabalin (PGN) in bulk and pharmaceutical formulations. The method was based on the production of a colored complex by reacting PGN with ascorbic acid in DMSO solvent. The resultant complex exhibits absorption maxima at 390 and 532 nm. The factors that affect the complex development and stability were studied and optimized. The reaction stoichiometry of drug: reagent was found to be 1:2. The method was then validated according to ICH guidelines. Regression analysis of Beer's plot showed good correlation (r2 value more than 0.998) within a concentration range of 5-30μg/ml. Linearity was confirmed by standardized residuals versus fitted value plots using Minitab14 software. The limits of detection and quantification at 390 and 532nm were 1.34μg/ml, 1.09μg/ml and 4.05μg/ml, 3.294μg/ml, respectively. Added recovery measurements were found to be 100.04±2.07% and 99.58 ±1.98% at 390nm and 532nm, respectively, which reflect the accuracy of the method and freedom from interference (relative standard deviation values were less than or equal 0.2%). The average assay for the commercial capsule preparation (PGN 150mg/capsule) was found to be 101.373±0.49 and 101.812±0.73 at 390 and 532nm, respectively. The developed method is an inexpensive, extraction free and can be applied for routine analysis of PGN in most of analytical laboratories.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

scholarly journals Spectrophotometric flow injection procedure to indirect determination of paracetamol in pharmaceutical formulations using o-tolidine as reagent

2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Flow Injection ◽  
Pharmaceutical Formulations ◽  
Injection Method ◽  
Indirect Determination ◽  
Analytical Curve ◽  
Relative Standard ◽  
Injection Procedure

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

scholarly journals A sensitive spectrophotometric determination of tadalafil in pharmaceutical preparations and industrial wastewater samples

2013 ◽  
Vol 10 (3) ◽  
pp. 1005-1013 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Standard Deviation ◽  
Industrial Wastewater ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Average Recovery ◽  
Relative Standard ◽  
Wastewater Samples ◽  
Sensitive Spectrophotometric Method

A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations (tablets) and industrial wastewater samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of tadalafil in true samples.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

Determination of cis,cis-Methylene Interrupted Polyunsaturated Fatty Acids in Fats and Oils By Capillary Gas Chromatography

1986 ◽  
Vol 69 (1) ◽  
pp. 65-67
Author(s):  
Albert K Athnasios ◽  
Edward J Healy ◽  
Anthony F Gross ◽  
Gareth J Templeman
Keyword(s):  
Fatty Acids ◽  
Polyunsaturated Fatty Acids ◽  
Fatty Acid Methyl Esters ◽  
Capillary Column ◽  
Methyl Esters ◽  
Fats And Oils ◽  
Pufa Content ◽  
Acid Methyl ◽  
Relative Standard

Abstract A capillary gas chromatographic (CGC) method is described for the determination of cis,cis-methylene interrupted polyunsaturated fatty acids (cis-PUFA) in fats and oils. The sample is saponified and the liberated fatty acids are esterified to the corresponding methyl esters. The latter are analyzed by CGC using a 60M SP2340 capillary column. Area percent values for 9,12-cis,cis-C18:2 and 9,12,15-cis,cis,cis-C18:3 fatty acid methyl esters are summed to give the total cis-PUFA content. Gas chromatographic results agreed well with those obtained by an enzymatic lipoxygenase method at the 31-48% cis-PUFA levels with a correlation coefficient of 0.98. The method has a precision (relative standard deviation) of 0.33% at a 44.4% cis-PUFA level in margarine oil.

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