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.