毛细管气相色谱法测定CHU-9126中有机溶剂残留量

Determination of Organic Solvents Residual in CHU-9126 by Capillary Gas Chromatography

建立CHU-9126中3种有机溶剂残留量的测定方法。使用毛细管气相色谱仪,采用DB-624毛细管色谱柱(94%二甲基聚硅氧烷和6%氰丙基苯聚硅氧烷);柱温70℃,保持3分钟;以3℃·min-1的速度升温至90℃,保持7分钟;以20℃·min-1的速度升温至220℃,保持3分钟。以氮气为载气,流速为2ml·min-1;FID检测器。乙醇,四氢呋喃和N,N-二甲基甲酰胺线性关系良好;平均回收率分别为99·9%,100·3%,99·6%;检出限分别为0·12ng,0·10ng,0·28ng。本方法简便,灵敏度高,重复性好,结果准确,适合于CHU-9126中有机溶剂残留量的测定。

A gas chromatographic method for determination of organic solvents residual in CHU -9126 was established. A DB -624 capillary gas chromatographic column coated with 94% dimethylpolysiloxane and 6% -1 cyanopropylpolysiloxane stationary phase was used with the carrier gas of nitrogen at a flow rate of 2ml·min^-1. The initial column temperature was kept at 70℃ for 3 minutes, then raised to 90℃ at the rate of 3℃·min^-1 and kept for 7 minutes, then raised to 220℃ at the rate of 20℃·min^-1. There were good relationship between the area and amounts of ethanol, tetrahydrofuran and N, N - dimethylformamide. The average recovery rates were 99.9%, 100.3% and 99. 6%, and limit of detection were 0. 12, 0. 10 and 0. 28ng respectively. This method appeared to be sensitive, accurate, repeatable and easy to operate.