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研究建立了固相萃取-高效液相色谱-电感耦合等离子体质谱联用技术(SPE-HPLC-ICPMS)测定水产品中游离态三价铝(Al3+)的提取、净化及检测方法.选用CG5A阳离子保护柱和CS5A阳离子分析柱对样品中Al3+进行分离,流动相组成为0.040 mol/L LiOH,0.0060 mol/L吡啶-2.6-二羧酸(PDCA)和0.090 mol/L CH3COOH(pH 4.7);用流动相做提取剂,将样品置70℃恒温水浴振荡器浸提2 h,浸提液经离心后,上清液用Oasis MCX(3 mL/60 mg,30 m)固相萃取柱净化,固相萃取柱使用前用2 mL甲醇和4 mL去离子水活化和平衡,2 mL 0.075 mol/L的HCL溶液洗脱目标组分.该提取净化方法能有效排除水产品中有机质的干扰,提高方法灵敏度.新建方法的回收率>89%,相对标准偏差<5%.采用本方法对样品中Al3+的检测结果与化学试剂浸提法的分析结果一致.
The extraction, purification and determination of free trivalent aluminum (Al3 +) in aquatic products by solid-phase extraction coupled with high performance liquid chromatography-inductively coupled plasma mass spectrometry (SPE-HPLC-ICPMS) The mobile phase consisted of 0.040 mol / L LiOH, 0.0060 mol / L pyridine-2,6-dicarboxylic acid (PDCA) and 0.090 mol / L CH3COOH (pH 4.7) Phase extraction solvent, the sample was set at 70 ℃ constant temperature water bath oscillator for 2 h, the extract was centrifuged, the supernatant with Oasis MCX (3 mL / 60 mg, 30 m) solid phase extraction column purification, solid phase The extraction column was activated and equilibrated with 2 mL of methanol and 4 mL of deionized water before use, and 2 mL of 0.075 mol / L HCL solution was used to elute the target components.The extraction and purification method can effectively eliminate the interference of organic matter in aquatic products and improve the method sensitivity The recovery rate of the new method was> 89% and the relative standard deviation was less than 5%. The results of Al3 + in this method were consistent with the results of chemical reagent extraction.