ISSN

0974-4150 (Online)
0974-4169 (Print)


Author(s): Perla Ganesh, CH. B. V. Narasimha Raju, N. Jagadeesh, Hemant M. Gandhi, BM. Rao, Dharamasoth Rama Devi, K. Basavaiah

Email(s): pganesh168@gmail.com

DOI: 10.52711/0974-4150.2024.00005   

Address: Perla Ganesh1,3*, CH. B. V. Narasimha Raju1,3, N. Jagadeesh1, Hemant M. Gandhi1, BM. Rao3, Dharamasoth Rama Devi2, K. Basavaiah3
1Dr. Reddy’s Laboratories Limited, API Plant, Bollaram - III, Plot No 116, IDA Bollaram, Medak District, Hyderabad 502325, Telangana, India.
2Dr. Samuel George Institute of Pharmaceutical Sciences, Markapur, India.
3Department of Chemistry, Andhra University, Vishakhapatnam, India.
*Corresponding Author

Published In:   Volume - 17,      Issue - 1,     Year - 2024


ABSTRACT:
The study aimed to develop and validate the method for trace level analysis of 2-(3-(trifluoromethyl)phenyl)propanal (2-TFL) impurity in calcium sensing receptor drugs by gas chromatographic method using mass spectrometry (GC-MS). The method utilizes a capillary column with 6% cyanopropyl phenyl and 94% dimethylpolysiloxane stationary phase with EI source in Selective Ion Monitoring (SIM) mode under programming temperature was used. After successful development, the method was validated according to our in-house validation guidelines for trace level analysis. The method proved to be selective for 2-(3-(trifluoromethyl) phenyl)propanal impurity in drug substance. A dissolve and injection approach was adopted for sample introduction in a split mode. Methanol was used as a diluent. The calibration curves showed good linearity over the concentration range from 1.85 (LOQ to 5.56ppm (150%)) of the target concentration of 3 ppm. The correlation coefficient obtained was >0.999. A limit of detection (LOD) of about 0.56ppm was achieved and limit of quantitation (LOQ) of 1.85ppm was achieved for 2-(3-(trifluoromethyl)phenyl)propanal impurity, when the samples were prepared at 20mg/mL. While recovery proved to be 101.0% at Limit of quantification (LOQ) level, 102.1% at Target analytical level (TAL) and 98.1% at 150% of the TAL, demonstrate the absence of matrix effect.


Cite this article:
Perla Ganesh, CH. B. V. Narasimha Raju, N. Jagadeesh, Hemant M. Gandhi, BM. Rao, Dharamasoth Rama Devi, K. Basavaiah. Trace level Determination of 2-(3-(trifluoromethyl)phenyl)propanal in Calcium Sensing Receptor drug by GCMS. Asian Journal of Research in Chemistry. 2024; 17(1):25-0. doi: 10.52711/0974-4150.2024.00005

Cite(Electronic):
Perla Ganesh, CH. B. V. Narasimha Raju, N. Jagadeesh, Hemant M. Gandhi, BM. Rao, Dharamasoth Rama Devi, K. Basavaiah. Trace level Determination of 2-(3-(trifluoromethyl)phenyl)propanal in Calcium Sensing Receptor drug by GCMS. Asian Journal of Research in Chemistry. 2024; 17(1):25-0. doi: 10.52711/0974-4150.2024.00005   Available on: https://ajrconline.org/AbstractView.aspx?PID=2024-17-1-5


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