Quantitative analysis of sitagliptin using the (19)F-NMR method: a universal technique for fluorinated compound detection.
To expand the application scope of nuclear magnetic resonance (NMR) technology in quantitative analysis of pharmaceutical ingredients, (19)F nuclear magnetic resonance ((19)F-NMR) spectroscopy has been employed as a simple, rapid, and reproducible approach for the detection of a fluorine-containing model drug, sitagliptin phosphate monohydrate (STG). ciprofloxacin (Cipro) has been used as the internal standard (IS). Influential factors, including the relaxation delay time (d1) and pulse angle, impacting the accuracy and precision of spectral data are systematically optimized. Method validation has been carried out in terms of precision and intermediate precision, linearity, limit of detection (LOD) and limit of quantification (LOQ), robustness, and stability. To validate the reliability and feasibility of the (19)F-NMR technology in quantitative analysis of pharmaceutical analytes, the assay result has been compared with that of (1)H-NMR. The statistical F-test and student t-test at 95% confidence level indicate that there is no significant difference between these two methods. Due to the advantages of (19)F-NMR, such as higher resolution and suitability for biological samples, it can be used as a universal technology for the quantitative analysis of other fluorine-containing pharmaceuticals and analytes.
State Key Laboratory of Natural Medicines, Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China. ayanju@163.com.
Fen-Fen
FF
Zhang
Meng-Hong
MH
Jiang
Lin-Lin
LL
Sun
Feng
F
Zheng
Lei
L
Dong
Vishva
V
Shah
Wen-Bin
WB
Shen
Ya
Y
Ding
D005461:Fluorine / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy; D011719:Pyrazines / Q000032:analysis*; D000068900:Sitagliptin Phosphate; D014230:Triazoles / Q000032:analysis*
D011719:Pyrazines; D014230:Triazoles; D005461:Fluorine; D000068900:Sitagliptin Phosphate