Development and validation of the method for the detection of glimepiride via derivatization employing N -methyl- N -(trimethylsilyl) trifluoroacetamide using gas chromatography-mass spectrometry

Egyptian Journal of Forensic Sciences

article

Verma, Priyanka¹  Bajaj, Atul²  Tripathi, R. M.²  Shukla, Sudhir K.¹  Nagpal, Suman³ 

[1] Amity Institute of Forensic Sciences, Amity University;Central Forensic Science Laboratory;Amity Institute of Advanced Research and Studies (Material and Devices), Amity University

关键词: Diabetes mellitus;    Glimepiride;    MSTFA;    Derivatization;    Gas chromatography-mass spectrometry;    Biological matrices;   

DOI  :  10.1186/s41935-021-00217-7

学科分类：心脏病和心血管学

来源: Springer

【 摘 要 】

Recent advances in the diversified anti-diabetic drugs have appeared in the startling increase in the count of poisoning cases. The epidemics of diabetes mellitus are increasing; hence, the no. of anti-diabetic drug users raised by 42.9%. The use of glimepiride raised to 24%. As the toxicity and drug cases are also escalating with increasing epidemics of diabetes mellitus, a novel gas chromatography-mass spectrometry (GC-MS) method for detecting glimepiride in biological matrices is developed. Liquid-liquid extraction method was employed by using 1-butanol: hexane (50:50, v/v) under an alkaline medium, and then back extraction was done via acetic acid. Distinct derivatization techniques were employed for the sample preparation for GC-MS analysis, i.e., silylation and acylation. Derivatization approaches were optimized under different parameters, i.e., reaction temperature and reaction time. N-Methyl-N-(trimethylsilyl) trifluoroacetamide [MSTFA] was found to be the best sound derivatization reagent for the GC-MS analysis of glimepiride. Total ion current (TIC) mode was selected for the monitoring of ions of trimethylsilyl (TMS) derivative of glimepiride with an m/z ratio of 256. Distinct parameters like specificity, carryover, stability, precision, and accuracy were evaluated for validating the identification method. The GC-MS method is found to be linear and illustrated within the range 500 to 2500 ng/ml with the value of R2 (coefficient of determination) at 0.9924. The stability of the extracted and derivatized glimepiride was accessed with regard to processed/extracted sample conditions and autosampler conditions, respectively. Accuracy at each concentration level was within the + 15% of the nominal concentration. Precision (%) for the interday and intraday analysis was found to be in the respectable spectrum. Henceforth, the proposed GC-MS method can be employed for the determination of glimepiride in biological matrices.

【 授权许可】

CC BY