scholarly journals A Validated GC-MS Method for the Determination of Genotoxic Impurities in Divalproex Sodium Drug Substance

2018 ◽  
Vol 57 (2) ◽  
pp. 101-107
Author(s):  
S Raghavender Reddy ◽  
K Hussain Reddy ◽  
M Narendra Kumar ◽  
P Madhava Reddy ◽  
J Venkata Ramana Reddy ◽  
...  
Keyword(s):  
Drug Substance ◽  
Divalproex Sodium ◽  
Genotoxic Impurities

scholarly journals An efficient HILIC-MS/MS method for the trace level determination of three potential genotoxic impurities in aripiprazole active drug substance

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Sumanth Mullangi ◽  
Kunta Ravindhranath ◽  
Ravi Kiran Panchakarla
Keyword(s):  
Mobile Phase ◽  
Active Drug ◽  
Gradient Elution ◽  
Drug Substance ◽  
Hydrophilic Interaction ◽  
Chromatography Tandem Mass Spectrometry ◽  
Genotoxic Impurities ◽  
Liquid Chromatography Tandem Mass ◽  
Gradient Elution Mode

AbstractA sensitive and selective hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method was developed and validated for trace analysis of potential genotoxic impurities (PGIs): 2,3-dichloroaniline (PGI-1), bis(2-chloroethyl) amine (PGI-2), and 2-chloroethylamine (PGI-3), in aripiprazole (APZ) active drug substance. Separation of analytes was achieved on ACE HILIC–N Column (HILN-5-1046U, 100 × 4.6 mm, 5 μm) in gradient elution mode with mobile phase A [acetonitrile:ammonium formate buffer (95:5 v/v)] and mobile phase B [acetonitrile:ammonium formate buffer (50:50 v/v)] at a flow rate of 0.8 mL/min. Developed method was linear in the concentration range of 8–100 ppm for PGI-1, 11–100 ppm for PGI-2, and 12.5–100ppm for PGI-3 with R2 > 0.996. The developed method was accurate for quantification of each PGI with percent recoveries greater than 96% and RSD (%) not more than 5%. The developed method was precise for quantification of PGIs in aripiprazole with RSD (%) of not more than 4% for any of the PGIs. There was no interference of diluent peaks at the retention time of the PGIs and APZ in the method. All the PGIs and sample solutions were found to be stable at ambient laboratory temperature (25 ± 5 °C) and refrigerated condition (2–8 °C) for a period of 48 h. The developed HILIC-MS/MS method can be used for trace quantification of PGIs in aripiprazole drug in quality control laboratories of the pharmaceutical industry.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

scholarly journals Low Level Quantification of Potential Genotoxic Impurities In Telmisartan Drug Substance by HPLC

2021 ◽  
Vol 11 (3) ◽  
pp. 24-35
Author(s):  
K. Srivalli ◽  
N. Annapurna ◽  
K. Raghu Babu ◽  
C. Ramdas ◽  
Hemant Kumar Sharma ◽  
...  
Keyword(s):  
Drug Substance ◽  
Low Level ◽  
Genotoxic Impurities

scholarly journals A SELECTIVE AND SENSITIVE LC-MS/MS METHOD FOR QUANTIFICATION OF FOUR POTENTIAL GENOTOXIC IMPURITIES IN ATAZANAVIR SULFATE DRUG SUBSTANCE IN TRACE LEVEL

2021 ◽  
pp. 137-144
Author(s):  
SIVA JYOTHI N. ◽  
VENKATNARAYANA MUVVALA
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Research Work ◽  
Active Pharmaceutical Ingredient ◽  
Drug Substance ◽  
Genotoxic Impurities ◽  
Liquid Chromatography Tandem Mass ◽  
Short Run ◽  
Acquity Uplc ◽  
Atazanavir Sulfate

Objective: The main objective of current research work is to develop and validate a rapid, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the trace analysis of four potential genotoxic impurities in Atazanavir Sulfate drug substance. Methods: LC-MS/MS analysis of four potential genotoxic impurities was done on Acquity UPLC CSH C18 (100 mm × 2.1 mm, 1.7 μm) column. In this method, mobile phase A (10 mM ammonium acetate) mobile phase B (methanol: acetonitrile (90:10, v/v) with gradient run with the flow rate of 0.2 ml/min. The method was developed with the short run time of 13 min. Triple quadrupole mass detector coupled with positive electrospray ionization was used for the quantification of genotoxic impurities in multiple reaction monitoring (MRM) mode. Results: The method was linear in the range of 0.3 ppm to 4.5 ppm for BOC Hydrazine Acid impurity, BOC Epoxide and Keto impurity with a correlation coefficient not less than 0.9994. The accuracy of the method was in the range of 99.26% to 105.71% for all four potential genotoxic impurities (PGIs). No impurities were identified in the Atazanavir Sulfate active pharmaceutical ingredient sample. Conclusion: The proposed method is specific, linear, precise, accurate, robust and stable for the quantification of the four genotoxic impurities at very low levels.

Determination of genotoxic impurities in pharmaceutical substances

2020 ◽  
Vol 69 (7) ◽  
pp. 10-16
Author(s):  
Olga Vyacheslavovna Ananyina ◽  
Mikhail Dmitrievich Khorolsky ◽  
Galina Vladislavovna Ramenskaya ◽  
Evgeniy Andreevich Zhukov ◽  
Natalia Viktorovna Maslennikova
Keyword(s):  
Pharmaceutical Substances ◽  
Genotoxic Impurities
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