摘要
建立了高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用测定多种生物样品中的无机汞和甲基汞的方法,并对比了提取生物样品中无机汞和甲基汞的不同前处理方法。实验使用5 mol/L的盐酸超声波提取样品中的无机汞和甲基汞。高效液相色谱流动相为含有0.06 mol/L醋酸氨,20μg/L B i,0.1%(V/V)2-巯基乙醇的5%(V/V)甲醇-水溶液,色谱柱为C18反相柱(5μm,3.9 mm×150 mm)。提取液在液相色谱中分离后,进入电感耦合等离子体质谱检测其中无机汞和甲基汞的浓度。测定了人发(GBW 07601),对虾(GBW 08572),鱼肉组织(IAEA MA-B-3/TM)和牛肝(GBW 080193)4种生物标准参考物,结果与标准参考物的标准值相符。无机汞和甲基汞检出限分别为0.3和0.2μg/L。
High performance liquid chromatography coupled with inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) has been developed for the determination of inorganic and methyl mercury in biological samples. Different techniques used to extract inorganic and methyl mercury from biological samples were also evaluated. The samples were sonicated to extract inorganic and methyl mercury in the system of 5 mol/L HCl. A 5 % (V/V) methanol-water mobile phase containing 0.06 mol/L ammonium acetate, 20 μg/L Bi and 0. 1% (V/V) 2-mercaptoethanol and a C18 reversed-phase column (5μm, 3.9 mm × 150 mm) was used for separation of CH3Hg^+ and Hg^2+ by HPLC. The concentrations of CH3Hg^+ and Hg^2+ in eluent were detected by ICPMS. Total four certified reference materials including human hair ( GBW 07601 ), prawn ( GBW 08572), fish (IAEA MA-B-3/TM) and bovine liver (GBW 080193) were analyzed. The results showed good accordance with the certified values. The detection limits of the method for inorganic and methyl mercury were 0.3 μg/L and 0.2 μg/L, respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第12期1671-1675,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金重大项目(No.10490181)
国家自然科学基金面上项目(No.204765055)
中国科学院重要方向性项目(No.KJCX2-N)
关键词
高效液相色谱
电感耦合等离子体质谱
联用技术
汞
生物样品
形态分析
High performance liquid chromatography, inductively coupled plasma-mass spectrometry, hyphened technique, mercury, biological samples, speciation analysis