顶空-气相色谱法同时测定芴类衍生物中4种残留溶剂的含量

Simultaneous Determination of Four Residual Solvents in Fluorene Derivatives by Headspace-Gas Chromatography

采用顶空-气相色谱法同时测定芴类衍生物中4种残留溶剂(甲醇、乙醇、1,4-二氧六环及甲苯)的含量。取芴类衍生物样品(0.5000g)置于20mL顶空瓶中,加入N,N-二甲基甲酰胺1mL溶解样品,立即将瓶密封。选择顶空平衡温度为100℃,平衡时间为30min,选择二苯基硅氧烷和二甲基硅氧烷以体积比5∶95的混合物作固定相的SE 54毛细管色谱柱作为分离柱,可达到上述4种溶剂的良好分离。用氢火焰离子化检测器,外标法定量。所得4种溶剂的标准曲线,甲醇和乙醇的线性范围均在8.0~800 mg·L-1之间,1,4-二氧六环及甲苯的线性范围在10.0~1000mg·L-1之间。其检出限(3S/N)依次为10.30,10.51,24.87,25.79μg·L-1。用标准加入法在3个浓度水平上进行回收试验,测得4种溶剂的回收率依次为99.4%,100%,101%和100%。

Headspace-gas chromatography was applied to the simultaneous determination of 4 residual solvents(i.e.,methanol,ethanol,1,4-dioxane and toluene)in fluorene derivatives.The sample(0.500 0 g)was placed into the 20 mL headspace flask and dissolved in 1 mL of N,N-dimethylformamide.The flask was then closed tightly.Equilibrium temperature and time taken for headspace sampling were 100 ℃ and 30 min.The capillary chromatographic column SE 54,using a mixture of diphenyl siloxane and dimethyl siloxane mixed by volume ratio of 5 to 95 as stationary phase was used as separation column on which the 4 solvents were separated clearly.Hydrogen flame ionization detector was adopted for detection and external standard method was used for quantification.Linearity ranges of the standard curves for methanol and ethanol were same between 8.0 to 800 mg·L-1,which for 1,4-dioxane and toluene were same between 10.0 to 1 000 mg·L-1,with limits of detection(3S/N)of 10.30,10.51,24.87,25.79μg·L-1 for the 4 solvents respectively.Test for recovery was made by addition of standards at 3 concentration levels,giving average recoveries of 99.4%(for CH3OH),100%(for C2H5OH),101%(for 1,4-dioxane)and 100%(for toluene).