气相色谱-质谱法测定异佛尔酮腈的氢氨化产物

Analysis of Hydroamination Products of Isophoronenitrile by GC-MS

采用GC-MS法对异佛尔酮腈氢氨化反应过程中生成的中间产物和主要副产物进行了结构分析,并对其可能的反应路径进行了推测,分析了杂质产生的主要原因;研究了反应体系中主要组分异佛尔酮、异佛尔酮腈、异佛尔酮亚胺和异佛尔酮二胺的GC分析方法,采用HP-5毛细管柱(30.0 m×320μm×0.25μm)和FID检测。实验结果表明,4组分的GC检测方法均具有良好的线性,线性相关系数R2=0.999 7～0.999 9,线性范围0.002～0.200 mg/mL,相对标准偏差均小于3.0%(n=4),平均加标回收率为99.6%～102.1%,定量限范围为0.001 5～0.054 6 mg/mL,检测限范围为0.000 35～0.007 60 mg/mL。该方法快速、准确、重现性高,可用于异氟尔酮腈氢氨化过程主要组分的定性、定量分析。

The structures of main intermediates and byproducts during the hydroamination of isophoronenitrile were analyzed. The possible reaction paths were inferred and the causes for the impurity generation were analyzed by means of GC-MS. A GC method for the analysis of the major components, namely isophorone, isophoronenitrile, isophoroneimine and isophoronelamine, in the reaction system was established with HP-5 capillary column（30.0μ m × 320 μm × 0.25 μm） and hydrogen flame ionization detector. The results show that the detection method has good linearity （R2=0.999 7-0.999 9 in the range of 0.002-0.200 mg/mL）. The standard deviations of the four compounds are less than 3.0%（n=4） with the average recoveries in the range of 99.6%-102.1%. The quantification limit and the detection limit are in the ranges of 0.001 5-0.054 6 mg/mL and of 0.000 35-0.007 60 mg/mL, respectively. The method is rapid, accurate and reproducible.