催化还原-管内固相微萃取-毛细管液相色谱系统用于二硝基芘同分异构体的分析

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

构建了催化还原-管内固相微萃取-毛细管液相色谱联用(CR-IT-SPME-CLC)体系,用于3种二硝基芘(DNP)同分异构体的快速分离分析。以Pt/Al 2O 3为催化剂,以甲酸铵为供氢体,在95℃的条件下,采用催化氢化的方法实现了3种DNP样品的高效还原。通过优化预聚合溶液组成,利用自制的毛细管旋转装置制备了还原氧化石墨烯均匀分布且渗透性良好的纳米材料共聚管内固相微萃取整体柱。优化了固相微萃取的解析液条件,实现了3种DNP还原产物二氨基芘的高效萃取,萃取效率可达82.48%~91.65%。以粒径为5μm的C 18为填料,采用高压匀浆填充法制备了毛细管色谱填充柱,并以此构建了毛细管液相色谱-激光诱导荧光检测(CLC-LIF)系统。通过优化色谱分离条件,在10 min内实现3种二氨基芘的完全分离。本方法操作简单、快速、灵敏,适合于硝基多环芳烃中DNP同分异构体的分析。

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/Al 2O 3 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 C 18 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.