Trace level Determination of 2-(3-(trifluoromethyl)phenyl)propanal in Calcium Sensing Receptor drug by GCMS

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...

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Bibliographic Details
Published in:Asian Journal of Research in Chemistry 2024-02, Vol.17 (1), p.25-30
Main Authors: Ganesh, Perla, Narasimha Raju, CH. B. V., Jagadeesh, N., M. Gandhi, Hemant, Rao, BM, Rama Devi, Dharamasoth, Basavaiah, K.
Format: Article
Language:English
Subjects:
Calcium
Chromatography
Drug dosages
Endocrine system
Gas chromatography
Homeostasis
Impurities
Laboratories
Liquid chromatography
Mass spectrometry
Methods
R&D
Receptors
Research & development
Scientific imaging
Solvents
Temperature
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Summary: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.
ISSN:0974-4169
0974-4150
DOI:10.52711/0974-4150.2024.00005