Citation: LI Ke, WANG Yu, YAN Yong, ZHAO Lei, ZHANG Dong-Tang, WANG Ya-Nan, GUO Guang-Sheng, WANG Xia-Yan. Catalytic Reduction-In-Tube Solid Phase Microextraction-Capillary Liquid Chromatography System for Analysis of Dinitropyrene Isomers[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(11): 1850-1856. doi: 10.19756/j.issn.0253-3820.191436 shu

Catalytic Reduction-In-Tube Solid Phase Microextraction-Capillary Liquid Chromatography System for Analysis of Dinitropyrene Isomers

Center of Excellence for Environmental Safety and Biological Effects, Beijing Key Laboratory for Green Catalysis and Separation, Department of Chemistry and Chemistry Engineering, Beijing University of Technology, Beijing 100124, China

Received Date: 22 July 2019
Revised Date: 17 September 2019

Fund Project: This work was supported by the National Natural Science Foundation of China(Nos.21804005, 21527808, 21625501) and the Beijing Municipal High Level Innovative Team Building Program, China (No. IDHT20180504).

In this study, a catalytic reduction-in-tube solid phase microextraction coupled with capillary liquid chromatography (CR-IT-SPME-CLC) system was developed for rapid analysis of dinitropyrene isomers (DNPs). Pt/Al₂O₃ and ammonium formate were used as catalyst and hydrogen donor respectively, and three DNPs were reduced efficiently by catalytic hydrogenation at 95℃. A solid phase microextraction monolithic column embedded into nanomaterial with uniform distribution of reduced graphene oxide and good permeability, which was prepared using self-made capillary rotating device by optimizing the composition of the pre-polymerization solution. For highly efficient extraction of three dinitropyrene reduction products, desorption solution of solid phase microextraction was optimized, and the extraction efficiency was 80.47%-93.37%. Capillary chromatography column was packed with C₁₈ particles (5 μm) at high chromatographic pump pressure, and a capillary liquid chromatography-laser induced fluorescence detection system was established. Complete separation of three diaminopyrenes was achieved in 10 min by optimizing the chromatographic separation conditions. The proposed method is simple, rapid and sensitive for the analysis of DNP isomers among nitropolycyclic aromatic hydrocarbons.
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