GC-MS测定磷酸西格列汀中基因毒性杂质水合肼 李善金.pdf

52 2 Vol. 52 52No. 2
第 卷第 期 method was established for the determination of the genotoxic impurity hydrazine hydrate in
Abstract：
Sitagliptin Phosphate. The detection was performed on DB-1701 (14%-cyanopropyl-phenyl) methyl polysiloxane
capillary column. The quantitative ion / 97 was scanned in the full scanning mode by derivatization using
m z
acetone and glacial acetic acid. The results showed that the hydrazine hydrate derivative in a test concentration
range between ng/mL to ng/mL had good linear relationship ( = 1). The quantification and
r
detection limits of the hydrazine hydrate derivative were ng/mL and ng/mL respectively. The average
recovery of the hydrazine hydrate derivative was 102%~112% , and a RSD ( =12) was less than 3%. The solution
n
used in the system was stable at 25 ℃ for 24 h with a RSD of less than 6%. The above method was applied in the
detection of three Sitagliptin Phosphate samples, and hydrazine hydrate derivative was not detected. The
established method is suitable for the determination of genotoxic impurity hydrazine hydrate in Sitagliptin
Phosphate wit