Separation of Cyclotetramethylenetetranitramine Synthetic Intermediates by Online Molecular Imprinted Solid Phase Extraction and Liquid Chromatography
10.11895/j.issn.0253-3820.140766
- VernacularTitle:分子印迹在线固相萃取分离奥克托今合成反应中间体
- Author:
Siyu WU
;
Min XUE
;
Jian WANG
;
Zihui MENG
- Publication Type:Journal Article
- Keywords:
Molecular imprinting technique;
Solid phase extraction;
High performance liquid chromatography-mass spectrometry;
Cyclotetramethylenetetranitramine
- From:
Chinese Journal of Analytical Chemistry
2014;(12):1767-1772
- CountryChina
- Language:Chinese
-
Abstract:
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.
