scholarly journals DEVELOPMENT OF ANALYTICAL METHOD FOR IMATINIB MESYLATE BY ULTRAVIOLET SPECTROSCOPY

2019 ◽  
pp. 180-183
Author(s):  
AJITHKUMAR P ◽  
ANTON SMITH A
Keyword(s):  
Imatinib Mesylate ◽  
Spectrophotometric Method ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Ultraviolet Spectroscopy ◽  
Limit Of Quantification ◽  
International Council ◽  
Technical Requirements ◽  
Human Use

Objective: A simple, selective, sensitive, specific, and spectrophotometric method has been developed for the detection of imatinib mesylate in pure form and formulations. Methods: The analytical condition was optimized for the drug, carried out as per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. Results: The drug shows absorption at 232.0 nm and obeyed beers law in the wide concentration range from 0.5 to 4.0 μg/ml. The lower limit of detection was found to be 0.331 μg/ml and the limit of quantification to be 1.004 μg/ml. The regression equation was found to be y = 0.08x. The precision of the method was found to be 99.04%±0.527% and the percentage of drug recovered by this method is 100.13%±1.375%. Conclusion: The method is simple and suitable for determination for imatinib mesylate in pure and pharmaceutical preparation.

scholarly journals Spectrophotometric method for determination of ranitidine hydrochloride in bulk and in pharmaceutical preparation using ninhydrin

2020 ◽  
Vol 11 (4) ◽  
pp. 291-297
Author(s):  
Hutaf Mustafa Baker ◽  
Hussam Ahmad Alsaoud ◽  
Hamzeh Mohamad Abdel-Halim
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Limit Of Quantification ◽  
Ranitidine Hydrochloride ◽  
Relative Standard ◽  
Reproducible Method

A simple, sensitive and reproducible method for the determination of ranitidine hydrochloride in pharmaceutical preparations was investigated. This spectrophotometric method was based on the formation of a deep red color product with ninhydrin in basic media and the absorbance measured at λmax = 480 nm. The reaction occurs at 45 °C with pH = 10 having a contact time of 38 minutes. Under the optimum conditions, Beer’s Law is obeyed in the concentration range of 8.98×103 - 9.90×104 µg/L. The coefficient of correlation was found to be 0.999 for the obtained method with molar absorptivity of 3.05×103 L/mol.cm. The calculated Sandell’s sensitivity is 0.108 μg/cm2. The limit of detection and limit of quantification are 0.0997 and 0.3023 µg/mL, respectively. The low values of the percentage relative standard deviation and percentage relative error indicate the high precision and the good accuracy of the proposed method. The stoichiometry of the reaction is determined and found to be 1:4 (Ranitidine hydrochloride:Ninhydrin). The initial rate method confirmed that this reaction is first order one.

scholarly journals A Validated Ion Chromatography method for determination of Ammonium content in Omeprazole tablets

2014 ◽  
Vol 2 (03) ◽  
pp. 90-95
Author(s):  
Swetha C. Parshaa ◽  
Y. Ravindra Kumara ◽  
M. Ravi Chanderb
Keyword(s):  
Detection Limit ◽  
Ion Chromatography ◽  
Limit Of Detection ◽  
Methane Sulfonic Acid ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Technical Requirements ◽  
Unknown Peak ◽  
Human Use

A simple, feasible, definite and strong Ion chromatography method was developed for the quantitative determination of ammonium content in Omeprazole tablets. The method was developed using Ion pac CS17 Column, 250 X 4.6mm X 5.0 m column with mobile phase containing 1.5mM Methane sulfonic acid in water. The eluted compounds were monitored using conductivity detector. The unknown peak and ammonium peak were well separated with resolution more than 2.0. The developed method was validated as per Internatonal Conference on Harmonisation of technical Requirements for registration of pharmaceuticals for human use guidelines with respect to linearity (The high correlation coefficient >0.99), limit of detection, limit of quantification, exactness, precision and robustness. The Limit of detection, Limit of quantification values of Ammonium were 8ppm and 30ppm respectively.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF HYDROQUINONE IN BULK, MARKETED CREAM AND PREAPARED NLC FORMULATION

2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Pure Form ◽  
Nanostructured Lipid Carrier ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.

Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

2020 ◽  
Author(s):  
Murat Soyseven ◽  
Rüstem Keçili ◽  
Hassan Y Aboul-Enein ◽  
Göksel Arli
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Detection System ◽  
Active Pharmaceutical Ingredient ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

scholarly journals Development of the UV Spectrophotometric Method of Azithromycin in API and Stress Degradation Studies

2016 ◽  
Vol 68 ◽  
pp. 48-53 ◽  
Author(s):  
Sandip Bhimani ◽  
Gaurav Sanghvi ◽  
Trupesh Pethani ◽  
Gaurav Dave ◽  
Vishal Airao ◽  
...  
Keyword(s):  
Linear Relationship ◽  
Spectrophotometric Method ◽  
Phosphate Buffer ◽  
Macrolide Antibiotic ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Limit Of Quantification ◽  
Absorbance Maximum ◽  
Antibiotic Drug ◽  
Stress Degradation

Azithromycin (AZI) is a semi-synthetic macrolide antibiotic drug, effective against a wide variety of bacteria. The present study describes a simple, accurate, reproducible and precise UV Spectrophotometric method for the estimation of AZI (pH 6.8 Phosphate buffer). The absorbance maximum (λmax) for AZI was found to be 208nm. The method reveals high sensitivity, with linearity in the 10 µg/ml to 50 µg/ml range. The lower limit of detection was found to be 1.6µg/ml and the limit of quantification was found to be 5µg/ml. All the calibration curves demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.99. The % recovery was found to be 99.72%. AZI was also subjected to stress degradation under different conditions recommended by the International Conference on Harmonization (ICH).

scholarly journals A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

2008 ◽  
Vol 33 (3) ◽  
pp. 7-12 ◽  
Author(s):  
M. A. Gotardo ◽  
L. S. Lima ◽  
R. Sequinel ◽  
J. L. Rufino ◽  
L. Pezza ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Coefficients Of Variation ◽  
The Common ◽  
Interday Precision ◽  
Sensitive Spectrophotometric Method

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

scholarly journals The importance of expert review to clarify ambiguous situations for (Q)SAR predictions under ICH M7

2020 ◽  
Vol 42 (1) ◽  
Author(s):  
Robert S. Foster ◽  
Adrian Fowkes ◽  
Alex Cayley ◽  
Andrew Thresher ◽  
Anne-Laure D. Werner ◽  
...  
Keyword(s):  
Quantitative Structure Activity Relationship ◽  
Quantitative Structure ◽  
Environmental Mutagen ◽  
International Council ◽  
Expert Review ◽  
Technical Requirements ◽  
Structure Activity ◽  
In Silico Predictions ◽  
Human Use ◽  
Selection Of

Abstract The use of in silico predictions for the assessment of bacterial mutagenicity under the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) M7 guideline is recommended when two complementary (quantitative) structure-activity relationship (Q)SAR models are used. Using two systems may increase the sensitivity and accuracy of predictions but also increases the need to review predictions, particularly in situations where results disagree. During the 4th ICH M7/QSAR Workshop held during the Joint Meeting of the 6th Asian Congress on Environmental Mutagens (ACEM) and the 48th Annual Meeting of the Japanese Environmental Mutagen Society (JEMS) 2019, speakers demonstrated their approaches to expert review using 20 compounds provided ahead of the workshop that were expected to yield ambiguous (Q)SAR results. Dr. Chris Barber presented a selection of the reviews carried out using Derek Nexus and Sarah Nexus provided by Lhasa Limited. On review of these compounds, common situations were recognised and are discussed in this paper along with standardised arguments that may be used for such scenarios in future.

scholarly journals Validation of a Thin-Layer Chromatography for the Determination of Hydrocortisone Acetate and Lidocaine in a Pharmaceutical Preparation

2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Katarzyna Kulpińska-Kucia ◽  
Alina Pyka
Keyword(s):  
Chromatographic Analysis ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Lidocaine Hydrochloride ◽  
Hydrocortisone Acetate ◽  
Limit Of Quantification ◽  
Bioactive Substances ◽  
Densitometric Detection ◽  
Layer Chromatography

A new specific, precise, accurate, and robust TLC-densitometry has been developed for the simultaneous determination of hydrocortisone acetate and lidocaine hydrochloride in combined pharmaceutical formulation. The chromatographic analysis was carried out using a mobile phase consisting of chloroform + acetone + ammonia (25%) in volume composition 8 : 2 : 0.1 and silica gel 60F254plates. Densitometric detection was performed in UV at wavelengths 200 nm and 250 nm, respectively, for lidocaine hydrochloride and hydrocortisone acetate. The validation of the proposed method was performed in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The applied TLC procedure is linear in hydrocortisone acetate concentration range of3.75÷12.50 μg·spot−1, and from1.00÷2.50 μg·spot−1for lidocaine hydrochloride. The developed method was found to be accurate (the value of the coefficient of variation CV [%] is less than 3%), precise (CV [%] is less than 2%), specific, and robust. LOQ of hydrocortisone acetate is 0.198 μg·spot−1and LOD is 0.066 μg·spot−1. LOQ and LOD values for lidocaine hydrochloride are 0.270 and 0.090 μg·spot−1, respectively. The assay value of both bioactive substances is consistent with the limits recommended by Pharmacopoeia.

scholarly journals Ultraviolet Spectrophotometric Method for Determination of Glipizide in Presence of Liposomal/Proliposomal Turbidity

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Neelkant Prasad ◽  
Roshan Issarani ◽  
Badri Prakash Nagori
Keyword(s):  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Clear Solution

A simple and sensitive ultraviolet spectrophotometric method for quantitative estimation of glipizide in presence of lipid turbidity is described to avoid false estimation due to diffraction by turbidity. UV detection was performed at 230 nm, 225 nm, and 235 nm, and the calibration curve was plotted between resultant of absorbance of [230 nm − (225 nm + 235 nm)/2] and concentration of analyte. The calibration curve was linear over the concentration range tested (1–20 μg/mL) with limit of detection of 0.27 μg/mL and limit of quantification of 0.82 μg/mL. Percent relative standard deviations and percent relative mean error, representing precision and accuracy, respectively, for clear as well as turbid solutions, were found to be within acceptable limits, that is, always less than 0.69 and 0.41, respectively, for clear solution and 0.65 and 0.47, respectively, for turbid solution. Conclusively, our method was successfully applied for the determination of glipizide in clear as well as turbid solutions, and it was found that the drug analyte in both types of solutions can be detected from the same calibration curve accurately and precisely and glipizide entrapped in the liposomes or in proliposomal matrix was not detected.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

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