毛细管气相色谱法测定萘哌地尔中的残留溶剂

GC Determination of Residual Solvents in Nafetoil

目的:建立气相色谱法分离测定萘哌地尔中的残留溶剂:乙醇、乙酸乙酯、氯仿、正丁醇、环氧氯丙烷。方法:以RX-5弹性石英毛细管柱为色谱柱(25m×0.32 mm),载气为氮气,采用氢离子火焰检测器,进样口温度为220℃,检测器为280℃,柱温采用程序升温,(60℃,保持4min,以10℃·min^(-1)升至100℃,并保持1min,再以25℃·min^(-1)升至220℃保持6 min),以二甲基亚砜为溶剂,进样量1μL。结果:乙醇、乙酸乙酯、氯仿、正丁醇、环氧氯丙烷的的进样量分别在25～400ng,其峰面积与浓度呈良好的线性关系,加样回收率(n=5)分别为99.47％(RSD<0.76％),99.03％(RSD<1.4%),97.91%(RSD<1.4%),97.90%(RSD<1.4%),98.02(RSD<1.4%),精密度良好。结论:本文气相色谱条件可用于同时测定萘哌地尔中乙醇、乙酸乙酯、氯仿、正丁醇、环氧氯丙烷的含量,方法简单准确。

Objective: This paper reports a GC method for determination of ethanol, ethyl acetate, chloroform, n - butanol and epichlorohydrin in nafetoil by GC. Method: Using a column RX -5, the column length was 25 m × 0. 32 mm. The injector temperature is 210℃. The detector temperature is 280℃. The column temperature is programmed raiced [60℃ (4 min) 100℃ (1 min) 220℃ (6 min) ]. The carri- er gas is nitrogen. The solvent was dimethyl sulfoxide. Results: The Standard curves are linear for ethanol, ethyl acetate, chloroform, n - butanol, epichlorohydrin in the range of 25 - 400 ng. The average recoveries ( n = 5 ) are 99. 5% (RSD<0. 76%) for ethanol, 99.0% (RSD<1.4%) for ethyl acetate, 97.9% (RSD<1.4%) for chloroform, 97. 9% (RSD < 1. 4% ) for n - butanol, 98. 0% ( RSD < 1. 4% ) for epichlorohydrin, respec-tively. Conclusion: This method is simple, rapid and precision.