Nguyen A L, Luong J H
Biotechnology Research Institute, National Research Council Canada, Montreal, Quebec, Canada, H4P 2R2.
Anal Chem. 1997 May 1;69(9):1726-31. doi: 10.1021/ac960986o.
A sensitive method for the determination of polycyclic aromatic hydrocarbons (PAHs) by solid phase microextraction coupled with cyclodextrin (CD)-modified capillary electrophoresis (CE) using UV detection has been developed. A glass fiber was prepared and used for absorbing 16 EPA priority PAHs from diluted samples until equilibrium was reached. After the glass fiber was connected to a separation capillary via an adapter, the absorbed analytes were directly released into the CE buffer stream, and electrophoretic separation was effected using a 50 mM borate, pH 9.2, buffer containing 35 mM sulfobutyloxy-β-CD, 10 mM methyl-β-CD, and 4 mM α-CD. Separation was effected since neutral PAHs differentially partitioned between the neutral and charged CD phases. Under 30 kV applied potential, separation was achieved in less than 15 min with high resolution and number of theoretical plates. Pyrene as low as 8 ppb was detected, while the highest limit of detection was 75 ppb for acenaphthene. Very satisfactory reproducibility with respect to migration time and peak area was obtained for repetitions using the same separation capillary and adapter, where only the extraction fiber was discarded after each analysis.
已开发出一种灵敏的方法，用于通过固相微萃取结合环糊精（CD）修饰的毛细管电泳（CE）并使用紫外检测来测定多环芳烃（PAHs）。制备了一根玻璃纤维，用于从稀释样品中吸收16种美国环境保护局（EPA）优先控制的PAHs，直至达到平衡。通过适配器将玻璃纤维连接到分离毛细管后，将吸附的分析物直接释放到CE缓冲液流中，并使用50 mM硼酸盐（pH 9.2）、含有35 mM磺丁基醚-β-环糊精、10 mM甲基-β-环糊精和4 mM α-环糊精的缓冲液进行电泳分离。由于中性PAHs在中性和带电的CD相之间存在差异分配，从而实现了分离。在30 kV的施加电压下，不到15分钟即可实现分离，具有高分辨率和理论塔板数。芘的检测限低至8 ppb，而苊的最高检测限为75 ppb。对于使用同一根分离毛细管和适配器的重复分析，在迁移时间和峰面积方面获得了非常令人满意的重现性，每次分析后仅丢弃萃取纤维。
