离子色谱-双阳极电化学氢化物发生-原子荧光光谱法测定Ⅰ型牙髓失活材料中的砷形态  

Ion Chromatography Coupled with Bi-anode Electrochemical Hydride Generation-Atomic Fluorescence Spectrometry for Determination of Arsenic Species in Dental Pulp Inactivative Agent Type Ⅰ

作　　者：申屠超[1,2] 侯逸众[3] 范云场[2] 朱岩[2] 

机构地区：[1]浙江树人大学生物与环境工程学院,杭州310015 [2]浙江大学理学院化学系,杭州310028 [3]桂林工学院材料与化学工程系,桂林541004

出　　处：《分析化学》2009年第2期263-266,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.20527005、20775070);浙江省自然科学基金(Nos.Y4080064、Z404105);浙江省钱江人才计划项目(No.2008R10028);浙江省分析测试基金(No.2008F70013)资助

摘　　要：将自制的双阳极电化学氢化物发生器作为离子色谱与原子荧光光谱的联用接口,建立了离子色谱-双阳极电化学氢化物发生-原子荧光光谱法在线分析砷形态系统。最佳实验条件为淋洗液6.0mmol/LNH4H2PO4(pH6.20),电解液0.40mol/LH2SO4,电解液流量为阳极4.0mL/min,阴极1.5mL/min,电解电流密度0.50A/cm2,载气流量300mL/min,屏蔽气流量500mL/min,氢气流量80mL/min。在优化的实验条件下,As(Ⅲ)、DMA、MMA的线性范围为5～200μg/L、As(Ⅴ)的线性范围为10～200μg/L,As(Ⅲ)、DMA、MMA和As(Ⅴ)检出限分别为3.04、4.27、3.97和9.30μg/L(信噪比S/N=3)。50μg/L的As(Ⅲ)、DMA、MMA和As(Ⅴ)混合标准溶液平行进样7次,得到的色谱峰面积的相对标准偏差(RSD)分别为4.15%、3.08%、5.19%和3.62%。将该方法用于牙髓失活材料中的砷形态分析。A novel method for the on-line determination of arsenic species by ion chromatography coupled with atomic fluorescence spectrometry using a home-made bi-anode electrochemical hydride generator as an interface（IC-BAECHG-AFS） has been investigated. Various experimental conditions and interference effects were examined. The optimal experimental conditions were as follows： eluent 6.0 mmol/L NH4H2PO4 （pH 6.20）, concentration of electrolyte （ H2SO4） 0.40 mol/L, electrolyte flow rate 4.0 mL/min in anode and 1.5 mL/min in cathode, electrolysis current density 0.50 A/cm^2, negative high voltage 290 V, flow rate of carrier gas 300 mL/min, flow rate of shield gas 500 mL/min and flow rate of hydrogen 80 mL/min. The linear ranges were 5 -200 μg/L for As（Ⅲ）, DMA and MMA and 10 - 200 Ⅲg/L for As（Ⅴ）. The limits of detection（ LOD, SIN =3） of As（Ⅲ）, DMA, MMA and As（Ⅴ） were 3.04 μg/L, 4.27 μg/L, 3.97 p4/L and 9.30 μg/L, respectively. The relative standard deviations （ RSD, n = 7, 50 μg/L for each） of peak area of As （Ⅲ）, DMA, MMA and As（Ⅴ） were 4.2% , 3.1% , 5.2% and 3.6% , respectively. The proposed method was also applied to the determination of arsenic species in dental pulp inactivative agent type Ⅰ. The spiked recoveries of As（Ⅲ）, DMA, MMA and As（Ⅴ） were 91.6% - 103.2%.

关 键 词：离子色谱 双阳极电化学氢化物发生 原子荧光光谱 Ⅰ型牙髓失活材料 砷形态 

分 类 号：R783.1[医药卫生—口腔医学]