UPLC-MS法测定磷酸西格列汀中的2种磷酸酯杂质的含量

Determination of 2 Phosphate Impurities in Sitagliptin Phosphate by UPLC-MS Method

建立了UPLC-MS法测定磷酸西格列汀中2种磷酸酯杂质含量的检测方法。采用C_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,0.01%甲酸和乙腈为流动相进行梯度洗脱,采用单极四级杆检测器,电喷雾离子源,正离子模式进行监测,外标法定量,分析方法时长13min。结果表明:该方法的线性关系相关系数r≥0.995;磷酸西格列汀样品加标回收率为82.05%~105.53%(n=9);磷酸三甲酯(TMP)检测限为0.0074μg·mL^(-1),磷酸三异丙基酯(TIP)检测限为0.0078μg·mL^(-1)。与常规高效液相方法相比,该方法简单快速,灵敏度高,准确度好,适用于磷酸西格列汀中磷酸三甲酯和磷酸三异丙基酯杂质的检测。

A UPLC-MS method for the determination of two phosphate impurities in sitagliptin phosphate was established.C_(18) chromatographic column(2.1mm×50mm,1.7μm)was used for separation,and 0.01%formic acid and acetonitrile were used to conduct gradient elution to the mobile phase.Single-pole quadrupole detector and electrospray ionization were used for monitoring under positive ion mode.And external standard method was used for quantification.The duration of this analysis method was 13 min.The results showed that the correlation coefficient of the linear relation in this method was r≥0.995;The adding standard recovery of the sitagliptin phosphate sample was 82.05%~105.53%(n=9);The detection limit of trimethyl phosphate(TMP)was 0.0074μg·mL^(-1),and that of triisopropyl phosphate(TIP)was 0.0078μg·mL^(-1).Compared with normal efficient liquid phase method,this method was easy,quick,has high sensitivity and good accuracy.This method was applicable to the detection of trimethyl phosphate and triisopropyl phosphate impurities in sitagliptin phosphate.