顶空毛细管气相色谱法测定奥格列汀中有机溶剂残留量  

Determination of residual organic solvents in omarigliptin by headspace gas chromatography

作　　者：郑飞[1] 华国栋[1] 项颖[1] 张彦丽[1] 张谦[1] 张超[1] 

机构地区：[1]北京中医药大学东方医院药学部,北京100078

出　　处：《安徽医药》2016年第10期1861-1864,共4页Anhui Medical and Pharmaceutical Journal

摘　　要：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 m L·min-1;取0.2 m L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10.06~2 012 mg·L^(-1)、10.10~2 020 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 another5 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 recoveries of ethanol,ethyl acetate and toluene were 97. 91%（ n = 9）,96. 48%（ n = 9）,and 95. 58%（ n = 9） respectively. Conclusions All the results demonstrate that this method is simple,reproducible and accurate enough for the determination of residual solvents in omarigliptin bulk drug.

关 键 词：奥格列汀原料药 有机溶剂残留 顶空气相色谱法 

分 类 号：R927.2[医药卫生—药学] O657.71[理学—分析化学]