Chen Jie, Huang Chaozhang, Hu Bin, Jiang Zucheng
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
J Agric Food Chem. 2004 Nov 17;52(23):6843-7. doi: 10.1021/jf049576o.
A technique using a flow injection microcolumn separation coupled with ICP-MS detection has been developed for the speciation of Al in drink samples. The retention behaviors of different Al species were studied with 8-hydroxyquinoline (8-HQ) loaded silylanization silica gel as the packing material and inorganic acid (HNO3) as the elution. The results indicated that in a pH range of 5.0 to 8.0, all labile monomeric Al species were retained on the microcolumn while nonlabile monomeric Al species were directly passed through the column. Various Al species after separation were detected by ICP-MS. The detection limit of 0.2 ng mL(-1) and a relative standard deviation (RSD) of 4.2% at 10 ng mL(-1) (n = 11) were achieved, and the recoveries for the spiked samples were 95-108%. The proposed method has been applied to the analysis of Al species in tea infusions, coffee, and tap waters with satisfactory results. The results obtained by this method were compared with that obtained by the cation exchange microcolumn separation and ICP-MS detection system, and some valuable conclusions were drawn.
已开发出一种采用流动注射微柱分离与电感耦合等离子体质谱（ICP-MS）检测相结合的技术，用于饮品样品中铝的形态分析。以负载8-羟基喹啉（8-HQ）的硅烷化硅胶为填充材料、无机酸（HNO₃）为洗脱剂，研究了不同铝形态的保留行为。结果表明，在pH值5.0至8.0范围内，所有不稳定的单体铝形态均保留在微柱上，而稳定的单体铝形态则直接通过柱子。分离后的各种铝形态通过ICP-MS进行检测。实现了0.2 ng mL⁻¹的检测限和10 ng mL⁻¹时4.2%的相对标准偏差（RSD）（n = 11），加标样品的回收率为95% - 108%。所提出的方法已应用于茶汤、咖啡和自来水中铝形态的分析，结果令人满意。将该方法获得的结果与阳离子交换微柱分离和ICP-MS检测系统获得的结果进行了比较，并得出了一些有价值的结论。
