Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus da Zapateira, Coruña, Spain.
J Chromatogr A. 2011 Jul 29;1218(30):4834-9. doi: 10.1016/j.chroma.2011.05.093. Epub 2011 Jun 6.
A new device for carbonyl compounds based on coupling on-line and miniaturizing both, sample pretreatment and chromatographic separation, is reported. Two capillary columns, a GC capillary column (95% methyl-5% phenyl substituted backbone, 70 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve for in-tube solid-phase microextraction (IT-SPME) and a Zorbax SB C18 (150 mm × 0.5 mm i.d., 5 μm particle diameter) LC capillary column were employed. Different combinations of IT-SPME and derivatization using 2,4-dinitrophenylhydrazine (DNPH) were examined for mixtures containing 15 carbonyl compounds (aliphatic, aromatic and unsaturated aldehydes and ketones). A screening analysis of aqueous extracts of atmospheric particulate PM(10) was carried out. Moreover, the possibility of coupling IT-SPME and conventional liquid chromatography is also tested. Derivatization solution and IT-SPME coupled to capillary liquid chromatography provided the best results for achieving the highest sensitivity for carbonyl compounds in atmospheric particulate analysis. Detection limits (LODs) using a photodiode array detector (DAD) were ranged from 30 to 198 ng L(-1), improving markedly those LODs reported by conventional SPME-LC-DAD.
本文报道了一种基于在线偶联和微型化的新型羰基化合物检测装置，该装置同时对样品预处理和色谱分离进行了微型化处理。在进样阀中采用了两根毛细管柱，一根为 GC 毛细管柱（95%甲基-5%苯基取代骨架，70cm×0.32mmID，3μm膜厚），用于管内固相微萃取（IT-SPME）；另一根为 Zorbax SB C18（150mm×0.5mmID，5μm粒径）LC 毛细管柱。本文考察了不同的 IT-SPME 和衍生化方法（使用 2,4-二硝基苯肼（DNPH））对包含 15 种羰基化合物（脂肪族、芳香族和不饱和醛和酮）的混合物的效果。对大气颗粒物 PM(10)的水提取物进行了筛选分析。此外，还测试了将 IT-SPME 与常规液相色谱法进行偶联的可能性。衍生化溶液和与毛细管液相色谱法偶联的 IT-SPME 为实现大气颗粒物分析中羰基化合物的最高灵敏度提供了最佳结果。使用光电二极管阵列检测器（DAD）的检测限（LOD）范围为 30 至 198ng/L，明显提高了常规 SPME-LC-DAD 报道的 LOD。
