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

• 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
• ISSN: 0974-4169; 0974-4150
• DOI: 10.52711/0974-4150.2024.00005

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.