以竹炭为固相萃取材料, 建立了顺序注射在线微填充柱固相萃取分离富集痕量铋的方法, 吸附在微填充柱上的铋(络合物）可用稀硝酸溶液(2.5 mol·L-1）洗脱回收。 洗脱液与硼氢化钠溶液混合进行氢化物发生(HG）反应, 氢化物经气液分离后与原子荧光(AFS）联用, 或直接将洗脱液引入电感耦合等离子体质谱(ICP-MS）, 实现了对生物及环境样品中痕量铋的高灵敏检测。 考察了固相萃取分离富集、 洗脱以及氢化物发生等过程中的影响因素。 当进样体积为1.0 mL时, 与HG-AFS联用测定铋的检出限为13 ng·L-1, 精密度为0.9%(0.3 μg·L-1, n=9）; 与ICP-MS联用的检出限为10 ng·L-1, 精密度为2.8%(0.3 μg·L-1, n=5）。 用标准物质CRM 320(河床沉积物）验证了方法的准确性, 并用两种检测方法分别对血液中的痕量铋进行了测定。 结果表明, 用原子荧光和等离子体质谱法测定铋所得到的结果无明显差异。

A procedure for the separation and preconcentration of bismuth was developed in a sequential injection system by employing bamboo carbon as sorbent. The detection was facilitated by both hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry. With a sample volume of 1 mL, a detection limit of 13 ng·L-1 was obtained, along with a precision of 0.9%(0.3 μg·L-1, n=9) with detection by HG-AFS, and a detection limit of 10 ng·L-1 along with a precision of 2.8% (0.3 μg·L-1, n=5) was achieved with detection by ICP-MS. The present system was validated by analyzing a certified reference material of river sediment (CRM 320), and spiking recovery of bismuth in human whole blood was performed with hydride generation atomic fluorescence spectrometry. No significant difference was identified in the results of bismuth detection in blood samples by hyphenating the present solid phase extraction system with detection by hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry.