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This paper presents a novel method for simultaneous online examination of free aluminum ions(Al3+)in seafood,using solidphase extraction and high-performance liquid chromatography online with inductively coupled plasma mass spectrometry(SPEHPLC-ICP-MS),without post-column reaction.The optimum conditions for chromatographic separation of Al3+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 CH3COOH(pH 4.7).The free Al3+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,30μm 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 Al3+were all above 89%and the relative standard deviations were all below 5%.The proposed method was successfully used for the examination of Al3+in seafood samples,and the results were similar to those obtained using the static equilibrium method.
This paper presents a novel method for simultaneous online examination of free aluminum ions (Al3 +) in seafood, using solid phase extraction and high-performance liquid chromatography online with inductively coupled plasma mass spectrometry (SPEHPLC-ICP-MS), without post-column reaction. The optimum conditions for chromatographic separation of Al3 + 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 CH3COOH (pH 4.7). The free Al3 + ions in seafood were extracted by shaking with the mobile phase at 70 ° C for 2 h. SPE was conducted using an Oasis MCX, 3 cc / 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 the inorganic Al from the SPE column. The standard recoveries of Al3 + were all above 89% and the relative standard deviations were all below 5%. proposed method wa s successfully used for the examination of Al3 + in seafood samples, and the results were similar to that obtained using the static equilibrium method.