振荡提取-高效液相色谱-电感耦合等离子体质谱法测定藻类中6种形态砷化合物  

Arsenic Speciation Analysis of Algae by Using Vibrated Extraction High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

作　　者：周志豪 黄振华[1] 周朝生[1] 陆荣茂[1] 曾国权[1] 陈星星[1] Zhou Zhihao;Huang Zhenhua;Zhou Chaosheng;Lu Rongmao;Zeng Guoquan;Chen Xingxing(Zhejiang Mariculture Research Institute,Zhejiang Key Laboratory of Exploitation and Preservation of Coastal Bio-resource,Wenzhou 325005,China)

机构地区：[1]浙江省海洋水产养殖研究所浙江省近岸水域生物资源开发与保护重点实验室,浙江温州325005

出　　处：《山东化工》2018年第21期71-73,76,共4页Shandong Chemical Industry

基　　金：石斑鱼哈维氏弧菌感染下噁喹酸给药处理及两者对肠道微生物影响的研究(LGN18C190006);海洋藻类中不同形态砷的测定方法及其应用(2016C37071);浙江省近岸水域重点实验室检测能力提升(2017F1022);温州地区表层沉积物中重金属元素分布特征及其污染评价(QS2017004)

摘　　要：建立一种同时测定藻类中6种形态砷化合物(亚砷酸根、砷酸根、一甲基砷酸、二甲基砷酸、砷甜菜碱、砷胆碱)的振荡提取-高效液相色谱-电感耦合等离子体质谱(high performance liquid chromatography-inductively coupled plasma mass spectrometry,HPLC-ICPMS)分析方法。选取0.3 mol/L乙酸溶液作为提取剂,振荡提取藻类样品中的砷化合物,选用阴离子交换柱,25 mmol/L磷酸二氢铵和水作为流动相进行梯度洗脱,经HPLC-ICP-MS进行分离和定量分析。结果表明,在优化实验条件下,6种形态砷化合物在0～50范围内线性良好,相关系数均在0.9960以上,检出限为0.24～0.34μg/L,相对标准偏差为3.00%～3.70%,加标回收率在之间85.1%～98.3%。4种处理方式后的藻类样品的测定结果显示,有机砷是主要的砷化物,占总砷含量的92.34%。方法灵敏度高,前处理简单高效,可以有效地分析藻类样品中不同形态的砷化物。The speciation of arsenic in algae was analyzed using vibrated extraction combined with high performance liquid chromatography - inductively coupled plasma mass spectrometry, HPLC - ICP - MS. Six arsenic compounds were extracted from the samples using 0. 3 mol/L acetic acid solution as extraction solvent. The chromatographic separation was performed on a hanfiton PRP- X100 anion exchange eolunm using a nfixture of 25 mmol/L amnloniunl dihydrogen phosphate and water as the mobile phase. Under the optinfized conditions, there were good linear relationships in the range of 0 -50μg/L for six arsenic species （ AsC, AsB, As III, DMA, MMA and As V ） were between 0.24 and 0.34 μg/L, the precision of the method, expressed as relative standard deviation（RSD） ,was less than 5%. The recoveries of AsC,AsB,As III, DMA,MMA and As V were in the range of 85.1% -98.3%. Speeiation analysis could accurately determine six arsenic species in algae. Organic arsenic was the main species in algae,which was in the range of 80.48% ~ 99%. this method was simple,rapid, sensitive and accurate, and could meet the requirements for the quantitative analysis of arsenic speeiation in algae.

关 键 词：砷 形态分析 振荡提取 高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS) 

分 类 号：O657.63[理学—分析化学]