| 郑飞,华国栋,项颖,等.顶空毛细管气相色谱法测定奥格列汀中有机溶剂残留量[J].安徽医药,2016,20(10):1861-1864. |
| 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 |
| 投稿时间：2016-06-13 |
| DOI： |
| 中文关键词: 奥格列汀原料药 有机溶剂残留 顶空气相色谱法 |
| 英文关键词: Omarigliptin Residual organic solvent Headspace GC |
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| 中文摘要: |
| 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×0.6 μm；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 ~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。 |
| 英文摘要: |
| 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 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. |
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