scholarly journals TRACE LEVEL DETERMINATION AND QUANTIFICATION OF POTENTIAL GENOTOXIC IMPURITIES IN DASATINIB DRUG SUBSTANCE BY UHPLC/INFINITY LC

2016 ◽  
Vol 8 (10) ◽  
pp. 209
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Elution Curve ◽  
Curve Number ◽  
Gradient Elution ◽  
Internal Diameter ◽  
Limit Of Quantification ◽  
Genotoxic Impurities ◽  
Test Concentration

<p class="Default"><strong>Objective: </strong>A simple, cost-effective and mass compatible ultra-high fast performance liquid chromatographic (Agilent-Infinity LC 1290) method has been developed and validated for the determination of potentially genotoxic impurities in dasatinib active pharmaceutical ingredients.</p><p class="Default"><strong>Methods: </strong>This method comprises the determination of three possible genotoxic impurities in dasatinib. The mobile phase is trifluoroacetic acid, acetonitrile and water with linear gradient elution curve number 6. The column used for the development and validation is zorbax RRHD eclipse plus C18 with the length of 50 mm, the internal diameter of 2.1 mm and particle size of 1.8 microns.</p><p class="Default"><strong>Results: </strong>The limit of detection of the potential genotoxic impurities are less than 0.1 µg/ml with respect to dasatinib test concentration of 1000 µg/ml. The limit of quantification of the potential genotoxic impurities is less than 0.3 µg/ml with respect to dasatinib test concentration of 1000 µg/ml.</p><p style="margin: 6pt 0cm; text-align: justify;"><strong>Conclusion: </strong>This method has been validated as per ICH guidelines Q2 (R1). These three potential mutagenic impurities are not degradant impurities of dasatinib and its only process related impurities. The method development has been approached using the QbD principle.</p>

scholarly journals Method Development and Validation for Simultaneous Determination of Ezetimibe and Simvastatin In Combined Pharmaceutical Dosage Form By RP-HPLC Method

2013 ◽  
Vol 2 (2) ◽  
pp. 60-69 ◽  
Author(s):  
G Krishnaveni ◽  
PVV Sathyannarayana
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Internal Diameter ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms

A simple, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of Ezetimibe and Simvastatin in bulk and pharmaceutical dosage forms. Chromatography was carried out by using Chromosil C-18,column having 250 x 4.6mm internal diameter with a mixture of Methanol:Acetonitrile:0.1%Orthophosphoric Aid in the ratio of 75:20:05 (v/v/v) as mobile phase. Determination of the different analytical parameters such as linearity, precision, accuracy, and specificity, limit of detection (LOD) and limit of quantification (LOQ) was done. The calibration curve was found to be linear for each analyte in the desired concentration range. The average recovery was found to be 99.88 and 100.12 for Ezetimibe and Simvastatin respectively. The proposed method is highly sensitive, precise and accurate, which was evident from the LOD value of 1.2ppm and 0.25ppm for Ezetimibe and Simvastatin respectively and hence the present method can be applied successfully for the quantification of active pharmaceutical ingredient (API) content in the combined formulations of Ezetimibe and Simvastatin. DOI: http://dx.doi.org/10.3329/ijpls.v2i2.15450 International Journal of Pharmaceutical and Life Sciences Vol.2(2) 2013: 60-69

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

scholarly journals UV-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF LORNOXICAM IN MICROSPONGES

2018 ◽  
Vol 10 (1) ◽  
pp. 74 ◽  
Author(s):  
Ayya Rajendra Prasad ◽  
Bannaravuri Thireesha
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Straight Line ◽  
Validation Parameters ◽  
Development And Validation

Objective: To develop and validate a novel, specific, precise and simple UV-spectrophotometric method for the estimation of lornoxicam present in microsponges.Methods: UV-spectrophotometric determination was performed with Thermo Scientific Evolution 201 UV-Vis spectrophotometer using methanol as a medium. The spectrum of the standard solution was run from 200-400 nm range for the determination of absorption maximum (λ max). λ max of lornoxicam was found at 353 nm. The absorbance of standard solutions of 3, 6, 9, 12 and 15, µg/ml of drug solution was measured at an absorption maximum at 353 nm against the blank. Then a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 3.0-15.0 µg/ml with a correlation coefficient of 0.9995. The limit of detection (LOD) and limit of quantification (LOQ) for lornoxicam was found at 1.26 μg/ml and 3.82 μg/ml respectively. Accuracy was in between 99.21 and 99.60%. % RSD for repeatability, intraday precision and interday precision were found to be 0.473, in between 0.478 and 0.619 and in between 0.855 and 1.818 respectively. The proposed UV method is found to be robust.Conclusion: The proposed UV-Visible spectrophotometric method was validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable and simple for the estimation of lornoxicam present in microsponges.

scholarly journals DETERMINATION OF RESIDUAL DIMETHYL SULFATE IN METHOXSALEN DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION WITH STATIC HEADSPACE GAS CHROMATOGRAPHY

2018 ◽  
Vol 10 (8) ◽  
pp. 84
Author(s):  
Ajit Anerao ◽  
Bhushan Patil ◽  
Nitin Pradhan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Sulfate ◽  
Drug Substance ◽  
Headspace Gas Chromatography ◽  
Limit Of Quantification ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Objective: Dimethyl sulfate has been highlighted as potential genotoxic and carcinogenic impurity. A sensitive Headspace gas chromatography (HS-GC) method with pre-column derivatization was developed and validated for the determination of dimethyl sulfate impurity in methoxsalen active pharmaceutical ingredient.Methods: HS-GC method on the column Agilent DB-5, 30m X 0.53 mm, film thickness 1.5 µm, with flame ionization detector (FID) was used. Derivatization reagent concentration, time of reaction and pH of the solution were optimized during method development. This analytical method was evaluated by performing method validation as per ICH guideline.Results: The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.5 μg/ml to 3.0 μg/ml and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) 2.0 μg/g and 5.0 μg/g respectively. Accuracy was observed within 98.1%–104.5%.Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of dimethyl sulfate impurity in methoxsalen drug substance.

scholarly journals Analytical method development and validation for the determination of Brinzolamide by RP-HPLC

2020 ◽  
Vol 10 (1) ◽  
pp. 92-96
Author(s):  
Balakrishna Tiwari ◽  
Mrunal K. Shirsat ◽  
Amol Kulkarni
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Uv Spectroscopy ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc

Brinzolamide is inhibitor of carbonic anhydride and is highly specific and non-competitive. The aim of the present study is to develop a simple, precise, accurate, sensitive RP-HPLC method for the determination of bulk drug. The objective of the method validation is to demonstrate whether the method was suited for the intended purpose. The method was validated as per the ICH guidelines. The method was validated for linearity, precision (repeatability, intermediate precision), accuracy, specificity, robustness, ruggedness, limit of detection and limit of quantification. Cosmosil (4.6X250mm, 5 μ) column was used for separation. The selected wavelength for Brinzolamide was 254 nm. The mobile phase consists of Acetonitrile: Potassium dihydrogen phosphate buffer (40:60). Flow rate was delivered at 1.0 mL/min. Appropriate dilutions of standard stock solutions were prepared to get desired concentrations in the range of 100-500 mcg/ml. The equation od standard curve was y = 441.8x + 1132 and R2 = 0.998. The RT obtained was 6.6167 minutes. Keywords: Brinzolamide, UV spectroscopy, RP-HPLC, ICH

scholarly journals Method Development for the Control of Potential Genotoxic Impurities in Vigabatrin Using Gas Chromatography Techniques and Mass Spectroscopy Detector

2021 ◽  
pp. 422-429
Author(s):  
D. Srikanth ◽  
S. Ganapaty ◽  
P. Manik Reddy ◽  
K. Sunitha ◽  
G. Sowjanya
Keyword(s):  
Method Development ◽  
Signal To Noise Ratio ◽  
Active Pharmaceutical Ingredient ◽  
Internal Diameter ◽  
Selected Ion Monitoring ◽  
Intermediate Precision ◽  
Quality Control Testing ◽  
Genotoxic Impurities ◽  
Headspace Gc

Aim: To develop a sensitive headspace GC-MS method for the determination of potential genotoxic impurities in Vigabatrin. Place and Duration of Study: The study was performed in SIONC Pharmaceuticals, Visakhapatnam from June 2020 to March 2021. Methodology: The impurities were determined by selected ion monitoring mode using VF -WAXms (30 mts length, 0.25 mm internal diameter, 1.0 µ film thickness) column. Helium gas was used as carrier gas with a column flow of 1.0 mL/min. and injector temperature maintained at 220 0C. Oven Temperature, loop temperature and transfer line temperature were maintained in the head space at 70oC, 90oC and 100oC respectively. Results: The linearity of the method was proposed in the range of LOQ to 150 % for the genotoxic impurities by subjecting the data obtained to statistical analysis using linear regression model (r2 > 0.99). The method also gave acceptable recovery of all the four impurities at each level and was found to be accurate. The % RSD obtained in the method precision and intermediate precision were less than 11% depicting the precision of the method. The LOD and LOQ values were calculated based on the signal to noise ratio and are indicating the sensitivity of the method. The specificity of the method was checked for blank interference at the retention time of respective impurities. Conclusion: The results proved that the proposed headspace GC-MS method for the study of potential genotoxic impurities of Vigabatrin was sensitive, precise and accurate and could be routinely used in the quality control testing of the active pharmaceutical ingredient.

scholarly journals Simultaneous determination of some illegal antihypertensive and diuretic drugs in traditional herbal preparations by HPLC-DAD

2021 ◽  
Vol 4 (2) ◽  
pp. 99-108
Author(s):  
Hung Pham Van ◽  
Son Tran Cao ◽  
Kieu Anh Nguyen Thi ◽  
◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Local Market ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Herbal Products ◽  
Herbal Preparations ◽  
Diuretic Drugs

A simple, stable, and specific high-performance liquid chromatography coupled with a&nbsp;DAD detector (HPLC-DAD) method has been developed and validated for the simultaneous&nbsp;determination of amlodipine, felodipine, furosemide, nifedipine, and spironolactone in&nbsp;traditional herbal products. The analytes were extracted in acetonitrile: water (50 : 50, v/v) with&nbsp;help of the ultrasonic. The separation of analytes was performed in an Apollo C18 column (250&nbsp;&times; 4.6 mm; 5 &mu;m) and a mobile phase consisting of mixture acetonitrile: 0.1% phosphoric acid in&nbsp;gradient elution. The analyzed drugs were detected at 238 nm. The method was validated according&nbsp;to the AOAC International guidelines concerning specificity, linearity, precision (repeatability,&nbsp;intermediate precision), accuracy, limit of detection (LOD), and limit of quantification (LOQ).&nbsp;The method can detect the studied drugs at the concentration of 0.66 to 1.25 &mu;g/g for dry&nbsp;samples and 0.10 to 0.24 &mu;g/mL for liquid samples. The method was successfully applied in the&nbsp;analysis of 17 samples in the local market. No samples were found positive for the substances to&nbsp;be analyzed.

scholarly journals Determination of Neonicotinoids in Honey Samples Originated from Poland and Other World Countries

Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5817
Author(s):  
Magdalena Ligor ◽  
Małgorzata Bukowska ◽  
Ileana-Andreea Ratiu ◽  
Renata Gadzała-Kopciuch ◽  
Bogusław Buszewski
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Pollen Grains ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Two Samples ◽  
Acacia Honey ◽  
Total Lack ◽  
Other World

A method development for determination of neonicotinoid residues in honey samples was developed. The proposed methodology consisted in QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe). That was used for sample preparation and UHPLC/UV (ultra-performance liquid chromatography with ultraviolet detection) utilized for chromatographic analysis. The developed method proved to be sensitive, with LOD (Limit of detection) value in the range of 60.80 to 80.98 ng/g hence LOQ (Limit of quantification) value was in the range of 184.26 to 245.40 ng/g. The method has tested on Polish honey and applied to honey from various countries (Bulgaria, Czech Republic, France, Greece, Italy, Portugal, Romania, Australia, Brazil, Cameroon, Russia, USA and Turkey). Several honey types were tested, while physicochemical properties of all honeys and were investigated. The methodology for general characterization of pollen grains originated from selected plants, to confirm the type of honey was also presented. There was a total lack of the mentioned neonicotinoids in sunflower honey. Except of this, only two samples of rapeseed and two samples of acacia honey (from Poland and Romania) were neonicotinoids free. In 19 samples the targeted pesticides were detected above LOQ. In all other investigated samples, the neonicotinoids were found at least at the LOD or LOQ level.

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