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 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 Separation and Determination of Process Related Impurities in Palbociclib: A Rp-hplc Study

2021 ◽  
pp. 485-499
Author(s):  
D. Srikanth ◽  
S. Ganapaty ◽  
P. Manik Reddy ◽  
G. Sowjanya ◽  
K. Sunitha
Keyword(s):  
Signal To Noise Ratio ◽  
Hplc Method ◽  
Forced Degradation ◽  
Intermediate Precision ◽  
Related Impurities ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Quality Control Testing ◽  
Gradient Mode

Aims: A new gradient RP-HPLC method was developed for the separation and determination of process related impurities in Palbociclib. Methodology: The chromatographic separation was achieved on a Inert sustain swift (C18) column using a mobile phase comprising of perchloric acid and acetonitrile in a gradient mode at a flow rate of 1 mL/min. over a runtime of 50 minutes. All the eluants were monitored at 230 nm. The optimized method was validated as per ICH guidelines for various parameters. Results: The linearity of the method was proposed in the range of LOQ to 250 % for the drug and its impurities by subjecting the data obtained to statistical analysis using correlation coefficient model (r > 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 2% 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 in the presence of process related impurities and also degradants generated by exposing to a variety of forced degradation conditions. Conclusion: The proposed RP-HPLC method for the determination of process related impurities of Palbociclib could be routinely used in the quality control testing.

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 DEVELOPMENT AND VALIDATION OF A TLC DENSITOMETRIC METHOD FOR DETERMINATION OF GLIMEPIRIDE IN TABLETS

2014 ◽  
Vol 16 (1) ◽  
pp. 11-15
Author(s):  
Yuni Retnaningtyas ◽  
Lestyo Wulandiri ◽  
Gabriella F Punu
Keyword(s):  
Pharmaceutical Analysis ◽  
Data Recovery ◽  
Antidiabetic Drug ◽  
Intermediate Precision ◽  
Quantification Limit ◽  
Accuracy And Precision ◽  
Quality Control Testing ◽  
The Mean ◽  
Development And Validation

A simple and valid TLC method has been developed for the determination of glimepiride in tablet formulation. After extraction of the analyte with a mixture of methanol and ammonia 0,2M (1:1, v/v), the extracts were spotted on precoated TLC silica gel F254 plates, which were developed with a mixture of toluene:methanol:ethyl acetate (75:20:5, v/v/v). Quantitative evaluation was performed by measuring the absorbance reflectance of the analyte spots at 238 nm. The method was validated for specificity, linearity, accuracy and precision. Good linearity was achieved in the concentration range 100–800 ng/spot. The RSD of repeatability and intermediate precision were found to be less than 2%, whereas the mean of the recovery data was 100-101%. The detection limit and quantification limit were 22 and 74 ng/spot, respectively. The method is specific, linear, precise, and accurate; it can be used for the routine quality control testing of marketed formulations.Keywords: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug Sebuah metode Kromatografi Lapis Tipis (KLT) yang sederhana dan valid telah dikembangkan untuk penentuan glimepiride dalam sediaan tablet. Setelah analit dalam sampel diekstraksi dengan campuran metanol dan amonia 0,2 M (1:1,v/v), ekstrak yang terlihat pada lempeng silika gel F254, yang dikembangkan dengan campuran toluen : metanol : etil asetat (75:20:5, v/v/v). Evaluasi kuantitatif dilakukan dengan mengukur reflektansi absorbansi noda analit pada panjang gelombang 238 nm.Metode ini divalidasi meliputi spesifisitas, linearitas, akurasi dan presisi.Linearitas yang baik dicapai pada rentang konsentrasi 100-800 ng / spot. RSD pengulangan dan presisi intermediate menunjukkan nilai kurang dari 2 %, sedangkan rata-rata data recovery adalah 100-101 % .Batas deteksi dan batas kuantifikasi adalah 22 dan 74 ng / noda.Metode ini spesifik, linear, tepat, dan akurat, bisa digunakan untuk pengujian kontrol kualitas rutin tablet glimepirid dipasarkan. Kata Kunci: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug

scholarly journals SIMULTANEOUS DETERMINATION OF 2-CHLORO METHYL PROPIONATE, 1,4-DI-BROMO BUTANE AND PARA ANISIC ALDEHYDE IN MEBEVERINE HYDROCHLORIDE API BY GAS CHROMATOGRAPHY-MASS SPECTROMETRIC WITH SELECTED-ION-MONITORING MODE

2016 ◽  
pp. 168
Author(s):  
Mannem Durga Babu ◽  
Surendrababu K ◽  
Uma Maheswar K
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Mass Spectrometric ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Selected Ion Monitoring ◽  
Methyl Propionate ◽  
Genotoxic Impurities ◽  
Pharmaceutical Industries

<p>ABSTRACT<br />Objective: To develop an accurate, precise and linear gas chromatography-mass spectrometric (GC-MS) selected-ion-monitoring (SIM) method for<br />quantitative estimation of 2-chloro methyl propionate (2-CMP), 1,4-dibromo butane and para anisic aldehyde (PAA) as an genotoxic impurities in<br />mebeverine HCl API (MEB) at ppm level and validated as per International Council of Harmonization (ICH) guidelines.<br />Methods: This method used in SIM mode mass selective detection was developed and validated for the trace level analysis of three impurities. All<br />these three impurities are simultaneously determined by a GC-MS method using VF-624 Capillary column (60 m×0.32 mm×1.80 µm) with Helium as<br />carrier gas and a flow rate of 2.0 mL/minutes. Chromatographic separation of 2-CMP, 1,4-DBB, and PAA was achieved in 7.91, 13.69, 18.45 minutes<br />and m/z values were 63, 55, 135 on SIM mode.<br />Results: The method was linear for 2-CMP, 1,4-DBB and PAA in mebeverine HCl 1.90 µg/ml to 7.5 µg/ml, respectively. The coefficient of correlation<br />(r<br />) for the 2-CMP, 1,4-DBB and PAA was better than 0.999. The limit of detection obtained was 0.28, 0.35, 0.22 µg/ml and the limit of quantification<br />(LOQ) obtained was 0.85, 1.06, 0.66 µg/ml. The method was fully validated, complying Food and Drug Administration, ICH and European Medicines<br />Agency guidelines. Furthermore, verified precision, accuracy, LOQ precision, LOQ accuracy, ruggedness, and robustness.<br />2<br />Conclusion: The proposed method is specific, accurate, precise, linear, rugged and robust for the determination of the three genotoxic impurities in<br />API of mebeverine HCl, and hence, is of wide applicability in pharmaceutical industries.<br />Keywords: 2-chloro methyl propionate, 1,4-dibromo butane, Para anisic aldehyde, Mebeverine HCl, Gas chromatography-mass spectrometric, Method<br />development, Method validation.</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

Sign in / Sign up

Export Citation Format

Share Document