尿中4种形态砷化物的离子色谱-氢化物发生-原子荧光光谱测定法  

Simultaneous Determination of Arsenic Species in Urine by Ion-Exchange Chromatography-Hydride Generation-Atomic Fluorescence Spectrometry

作　　者：李拥军[1] 苏福荣[1] 魏静[1] 倪霞[1] 

机构地区：[1]甘肃省疾病预防控制中心理化实验室,甘肃兰州730000

出　　处：《环境与健康杂志》2011年第9期809-811,共3页Journal of Environment and Health

摘　　要：目的建立尿中4种形态砷的离子交换色谱(IC)-氢化物发生(HG)-原子荧光光谱(AFS)联用测定法。方法尿样经过离心、0.22μm水系乙酸纤维素膜过滤两次,用阴离子交换分析柱,以15 mmol/L的(NH4)2HPO4溶液(pH=6.0)为流动相,盐酸浓度为0.07 g/ml,以15 mg/ml的KBH4-5 mg/ml的KOH为还原剂分离了亚砷酸[As(Ⅲ)]、砷酸[As(Ⅴ)]、一甲基胂酸(MMA)、二甲基胂酸(DMA),采用IC-HG-AFS进行测定。结果浓度在5～150μg/L范围内,所得四种形态砷的回归方程均呈较好的线性关系(r>0.999);As(Ⅲ)、DMA、MMA、As(Ⅴ)的检出限分别为0.8、1.7、1.3、3.6μg/L,平均回收率在74.5%～97.4%之间,RSD在1.8%～4.2%之间。结论该方法简便、快速,具有较好的精密度和准确度,适用于尿中4种形态砷的测定。Objective To develop a method for the determination of arsenic species in urine by ion-exchange chromatography-hydride generation-atomic fluorescence spectrometry （IC-HG-AFS）. Methods The samples of urine were centrifuged and filtered twice through the hydrocellulose acetate film （0.22μm）.The optimized mobile phase composition was 15 mmol/L （NH4）2HPO4（ 1.0 ml/min）,pH=6.0, and 1.5% KBH,-0.5% KOH（3.4 ml/min）as the reducer. Arsenite [As（ IH ）],arsenate [As （V）],monomethylarsonic acid （MMA） and dimethylarsinic acid （DMA） were separated and determinate by IC-HG-AFS. Results The peak areas were proportional to the arsenic species concentrations and the standard curve showed a good linearity within the range of 5-150μg/L （r=0.999）, average spiked recoveries for arsenite, DMA, MMA and arsenate were 74.5%-97.4%, relative standard deviations （n =6） were below 4.2%. The limits of detection were 0.8,1.7,1.3 and 3.6μg/L respectively. Conclusion This method is simple,fast,with a good separation effect, and is applicable to the determination of four arsenic soecies in urine.

关 键 词：色谱法 离子交换 氢化物发生 原子荧光光谱 尿 形态砷 

分 类 号：O657.7[理学—分析化学]