Fung Y S, Tung H S
Department of Chemistry, The University of Hong Kong, SAR, PR China.
Electrophoresis. 1999 Jul;20(9):1832-41. doi: 10.1002/(SICI)1522-2683(19990701)20:9<1832::AID-ELPS1832>3.0.CO;2-E.
A new buffer system consisting of 30 mM hydroxylamine hydrochloride, 0.1 mM 1,10-phenanthroline, 1% methanol and pH 3.7 was optimized for simultaneous determination of water and acid leachable metals from respirable, fine and coarse air particulate matters. A reducing environment was used to resolve metal ions with variable oxidation states. A suitable counteranion was employed to enable acidic pH to be used and methanol was added to improve the resolution of the electropherograms and to achieve simultaneous determination of several metal ions. Compared to existing capillary electrophoresis (CE) buffers, the buffer developed, based on direct UV detection of ion-pair with weak interaction, gives improved resolution and sharper, more stable and well-resolved peaks. It detects total irons and solves interfering problems due to the variable oxidation states of iron in environmental samples. Compared to existing mostly alkaline CE buffers for metal analysis, the acidic nature of the buffer system developed makes the pretreatment step simpler and reduces the risk of reagent contamination. Satisfactory working ranges (15-5500 ppb) and detection limits (0.5-3 ppb) were obtained for leachable Zn, Cu, Co, Fe and Cd. The NIST 1648 urban particulate matters were found to leach out 2.53-42.8% water-extractable and 2.76-71.7% acid-extractable Zn, Cu, Fe and Cd. High iron contents, and lower copper and zinc concentrations were found in respirable suspended particulates (RSP) sampled in Hong Kong.
一种由30 mM盐酸羟胺、0.1 mM 1,10 - 菲啰啉、1%甲醇和pH 3.7组成的新型缓冲体系,经优化用于同时测定可吸入、细颗粒和粗颗粒空气中颗粒物中的水溶态和酸溶态金属。采用还原环境来解析具有可变氧化态的金属离子。使用合适的抗衡阴离子以使酸性pH能够被采用,并加入甲醇以提高电泳图谱的分辨率,并实现几种金属离子的同时测定。与现有的毛细管电泳(CE)缓冲液相比,基于对具有弱相互作用的离子对进行直接紫外检测而开发的缓冲液具有更高的分辨率,峰形更尖锐、更稳定且分离良好。它能检测总铁含量,并解决环境样品中由于铁的可变氧化态而产生的干扰问题。与现有的大多用于金属分析的碱性CE缓冲液相比,所开发的缓冲液体系的酸性性质使预处理步骤更简单,并降低了试剂污染的风险。对于可溶态的锌、铜、钴、铁和镉,获得了令人满意的工作范围(15 - 5500 ppb)和检测限(0.5 - 3 ppb)。发现NIST 1648城市颗粒物中水溶态和酸溶态的锌、铜、铁和镉的浸出率分别为2.53 - 42.8%和2.76 - 71.7%。在香港采集的可吸入悬浮颗粒物(RSP)中发现铁含量高,而铜和锌浓度较低。