Development of a new method for analyzing free aluminum ions(Al^(3+)) in seafood using HPLC-ICP-MS  

作　　者：SHANG DeRong ZHAO YanFang ZHAI YuXiu NING JinSong DING HaiYan SHENG XiaoFeng 

机构地区：[1]Yellow Sea Fishery Research Institute, Chinese Academy of Fishery Sciences

出　　处：《Chinese Science Bulletin》2013年第35期4437-4442,共6页

基　　金：supported by the Agricultural Industry Standard of thePeople’s Republic of China(2011516);the National Natural Science Foundation of China(41206101);the Special Fund of Chinese General Government for Basic Scientific Research Operations in Commonweal Research Institutes(20603022012016);National Key Technology R&D Program of the Ministry of Science and Technology(2011BAD13B06)

摘　　要：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 （SPE- HPLC-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℃ 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 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.

关 键 词：铝离子 游离 海鲜 电感耦合等离子体质谱法 IonPac 高效液相色谱 相对标准偏差 固相萃取 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]