分子印迹在线固相萃取分离奥克托今合成反应中间体

摘要

An online solid phase extraction ( SPE ) coupled with high performance liquid chromatography (HPLC)-mass spectrometry (MS) method was developed for the separation of 1,3,5,7-tetraacetyl-1,3,5,7-tetraazacyclooctane ( TAT ) and 1 , 3 , 5-triacetyl-1 , 3 , 5-triazacyclohexane ( TRAT ) which are the synthetic intermediates of cyclotetramethylenetetranitramine ( HMX) . In this experiment, molecularly imprinted polymers with TAT as the template were used as SPE sorbents. PC HILIC column was employed in liquid chromatographic separation. The parameters of SPE-HPLC were optimized. Acetonitrile was selected as the loading solution with flow rate of 0. 1 mL/min. After flushed by ethyl acetate, the TAT adsorbed on SPE was eluted by methanol, which was also used as the mobile phase in HPLC separation. The mass spectrometry was coupled with HPLC to identify the corresponding peaks. Under the optimized conditions, the linear detection range of this method was 6. 0 mg/L to 500. 0 mg/L, with the detection limit of 1. 8 mg/L (3σ). The enriching factor was 400 times and TAT recovery was 79%–93% in the standard addition experiment.%采用分子印迹在线固相萃取和液相色谱-质谱联用技术建立了奥克托今合成反应中间体1,3,5,7-四乙酰基-1,3,5,7-四氮杂环辛烷(TAT)与1,3,5-三乙酰基-1,3,5-三氮杂环己烷(TRAT)的分离鉴定方法。固相萃取填料采用TAT分子印迹聚合物,液相色谱分离检测采用亲水色谱柱。首先以乙腈为固相萃取柱上样溶剂,流速为0.1 mL/min,然后以乙酸乙酯淋洗萃取柱,用甲醇洗脱,并以甲醇为流动相对洗脱溶液进行液相色谱分离,与质谱仪联用鉴定各分离组分。在上述条件下,TAT回收率在79％~93％,检出限为1.8 mg/L (3σ),线性范围为6.0~500.0 mg/L,富集倍数400倍。