目的：观察顶空毛细管气相色谱法（GC）测定奥格列汀原料药中乙醇、乙酸乙酯、甲苯3种残留溶剂的效果。方法采用 GC 法进行残留溶剂测定。色谱柱采用 DB-5弹性石英毛细管气相色谱柱，规格为50 m ×0．32 mm ×0．6μm；进样口温度为150℃，分流比1∶10；柱温程序为首先在40℃下保持6 min，再以每分钟15℃的速率升温至180℃；仪器配有氢火焰离子化检测器（FID），检测器温度为240℃；载气为高纯氮气，流速为恒流1 mL·min －1；取0．2 mL 顶部平衡气体进样。顶空条件为：N， N-二甲基甲酰胺（DMF）为溶剂，溶液浓度200 g·L －1，加热时间30 min，加热器温度100℃，传输线温度105℃。结果在相应色谱条件下，各残留溶剂均可基线分离。测得乙醇、乙酸乙酯、甲苯分别在10．06～2012 mg·L －1、10．10～2020 mg· L －1、1．78～356 mg·L －1范围内线性关系良好。乙醇、乙酸乙酯和甲苯的平均回收率分别为97．91％（n ＝9）、96．48％（n ＝9）、95．58％（n ＝9）。乙醇、乙酸乙酯、甲苯三种溶剂日内精密度 RSD 分别为2．13％（n ＝6）、4．84％（n ＝6）、5．41％（n ＝6），日间精密度 RSD 分别为1．98％（n ＝12）、4．51％（n ＝12）、5．09％（n ＝12）。结论GC 法操作简便、重现性好、结果准确可靠，可以用于奥格列汀原料药中残留溶剂的测定。%Objective To establish a method to determine residual solvents in omarigliptin bulk drug.Methods The headspace GC was performed with DB-5 capillary column with standard of 50 m ×0.32 mm ×0.6 μm.The condition of GC was as follows:the inlet temperature was 150 ℃;the injection volume was 0.2 mL with separation ratio of 1∶10;the column temperature was programmed with an initial temperature below 40 ℃,maintained for 6 min,then raised to 180 ℃ with a rate of 15 ℃·min -1 ,and maintained for another 5 min.The detector was equipped with FID with a temperature of 240 ℃.The carrying gas was N2 with the flow rate of 1 mL·min -1 . DMF was used as solvent for omarigliptin with the concentration of 200 g·L -1 .The solution was heated at 100 ℃ for 30 mins.The temperature of transferring line was 105 ℃.Results All solvents can be separated completely with good linear relationship in the range of 10.06 ~2 012 mg·L -1 (ethanol),10.10 ~2 020 mg·L -1 (ethyl acetate)and 1.78 ~356 mg·L -1 (toluene).The average re-coveries of ethanol,ethyl acetate and toluene were 97.91% (n =9),96.48% (n =9),and 95.58% (n =9)respectively.Conclu-sions All the results demonstrate that this method is simple,reproducible and accurate enough for the determination of residual sol-vents in omarigliptin bulk drug.
展开▼
