کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
1222063 | 1494659 | 2013 | 6 صفحه PDF | دانلود رایگان |

A new, simple and rapid gas chromatography–mass spectrometry (GC–MS) method for the determination of sitagliptin (STG) in human urine was developed and fully validated. STG was derivatized by N-methyl-trimethylsilyltrifluoroacetamide prior to GC–MS analysis and converted to its N-TMS amine derivative. It was extracted from urine by using carbonate buffer (pH 9.0) and ether. The method was validated in terms of specificity, limit of quantitation (LOQ), linearity, accuracy, precision, stability, recovery, robustness and ruggedness. LOQ was found to be 50 ng mL−1. The calibration curve was linear in the range of 50–600 ng mL−1 with a coefficient of determination (r2) above 0.997. The intra- and inter-day precisions were less than 8.76%, and the intra- and inter-day accuracies were found between 0.83 and 4.53%. The method was successfully applied to urine samples obtained from diabetic patients.
► A new and simple GC–MS method was developed for the analysis of Sitagliptin (STG) in human urine.
► Prior to analysis, STG was efficiently derivatized by using MSTFA.
► STG was extracted from urine with carbonate buffer (pH 9) and ether.
► After full validation of the method, it was successfully applied to the real human urine samples.
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 74, 23 February 2013, Pages 71–76