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

Abstract

Background 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. Results 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. Conclusion Henceforth, the proposed GC-MS method can be employed for the determination of glimepiride in biological matrices.

Novel Aspects of Gas Chromatography and Chemometrics

“…DOI: 10.1016/j.chroma.2009. 04.064 [69] Yang JJ, Han Y, Mah CH, Wanjaya E, Peng B, Xu TF, et al Streamlined MRM method transfer between instruments assisted with HRMS matching and retention-time prediction. Analytica Chimica Acta.…”

“…Instead, the group around Tolley and Lee concentrated on more theoretical studies on the separation behavior and simulation of GC separation under the different experimental conditions. These findings were published in a series of papers [68][69][70][71], many of which were based on the Master thesis of Avila published in 2021 [72]. They discuss in detail the simulation of capillary GC separations, including thermal gradient conditions [69], the comparison of static thermal gradient to isothermal conditions in GC [71] and the comparison of dynamic thermal gradient GC operation to temperature-programmed gas chromatography [71].…”

“…Later, Boeker and co-workers, in collaboration with Blumberg, also turned to the theoretical description and modelling of the TGGC separation. Notably the peak profiles and the separation performance of negative thermal gradient operation were discussed in a series of papers [83][84][85], which can be seen as a scientific dialog to the papers of Tolley and Lee [69][70][71]. This is particularly so as they were successfully describing both chromatographic separation and peak width.…”

“…In QSRR studies, the RF algorithm is readily used as a modeling technique [42,55,66,68] as well as a feature selection method [69,70]. The latter is due to the ability of the algorithm to quantify the importance of variables under study.…”

Quantitative determination of lobeglitazone sulfate and glimepiride in combined tablet by robust high‐performance thin layer chromatographic method

“…Ultraviolet spectrophotometry [15][16][17][18][19][20][21], highperformance liquid chromatography (HPLC) [22][23][24][25][26][27][28][29][30], high-performance thin-layer chromatography (HPTLC) [31][32][33][34][35][36][37], liquid chromatography-mass spectrometry (LC-MS) [38][39][40][41][42][43][44], and gas chromatography-mass spectrometry (GC-MS) [45] are among the analytical approaches stated in the literature for quantifying the concentrations of LBZ and GLM separately or in blend with other substances, in bulk drug samples or pharmaceutical formulations. Only two analytical methods have been reported [22,23] for determining LBZ individually, and these methods cannot be used to estimate the drugs in combined formulations.…”