This paper presents a novel method for simultaneous online examination of free aluminum ions (Al 3+ ) in seafood, using solidphase extraction and high-performance liquid chromatography online with inductively coupled plasma mass spectrometry (SPE-HPLC-ICP-MS), without post-column reaction. The optimum conditions for chromatographic separation of Al 3+ were achieved using an IonPac CS5A analytical column with an IonPac CG5A guard column. The mobile phase consisted of 0.040 mol/L LiOH, 0.0060 mol/L 2,6-pyridinedicarboxylic acid, and 0.090 mol/L CH 3 COOH (pH 4.7). The free Al 3+ ions in seafood were extracted by shaking with the mobile phase at 70°C for 2 h. SPE was conducted using an Oasis MCX, 3cc/60 mg, 30 μm column, which was activated and equilibrated with 2 mL of methanol and 4 mL of deionized water before use. HCl (0.075 mol/L, 2 mL) was used to wash inorganic Al from the SPE column. The standard recoveries of Al 3+ were all above 89% and the relative standard deviations were all below 5%. The proposed method was successfully used for the examination of Al 3+ in seafood samples, and the results were similar to those obtained using the static equilibrium method. Aluminum (Al) was long considered to be an innocuous element [1]. It was not until the discovery in the 1970s of its implication in "dialysis encephalopathy" syndrome, which affected hemodialysis patients, that attention was drawn to its possible deleterious effects [2]. Public interest in Al has therefore been increasing in the last few decades. The 67th report of the Joint FAO/WHO Expert Committee on Food Additives established a provisional tolerable weekly intake for Al of 1 mg/kg body weight, which applies to all Al compounds in food, including additives.Seafood (including fish, seaweed, shellfish, and sea cumber) is regarded as being a healthy and tasty food for humans, and human consumption of seafood in China has been increasing in recent decades. However, high concentrations of Al have been found in seafood, particularly seaweed, sea cucumber, and some shellfish. For example, the total Al concentration in seaweed is about 118-2715 mg/kg (dry weight) in Porphyra haitanensis and 340-1246 mg/kg (dry weight) in Laminaria japonica. In addition, the highest Al concentration in sea cucumber is about 1200 mg/kg (dry weight), and it is about 800 mg/kg (dry weight) in shellfish. There is therefore a serious problem with regard to the safety of seafood because of its high Al content, and this has attracted much attention. The current methods for determining the Al content of seafood almost all use concentrated acids, namely HNO 3 , HClO 4 and H 2 SO 4 , to achieve digestion of all forms of Al to Al 3+ , which is then measured using inductively coupled plasma mass spectrometry (ICP-MS) or ICP-atomic emission spectrometry (AES), so all the methods for determining the Al content of seafood measure the total Al.It is well known that Al can form complexes with various organic compounds (e.g. humic and fulvic acids, and lowmass organic compounds) and ino...