摘要
提出了一种用高效液相色谱(HPLC)分离和用电感偶合等离子体质谱仪(ICP-MS)或火焰原子吸收光谱仪(FAAS)作元素专一检测器在线测定硒的化学形态的方法。在优化的HPLC条件下,用ESAⅢ阴离子色谱柱(250mm×4.6mm),以柠檬酸铵为流动相(5.5mmol/L,pH5.5,流速1.5mL/min),进样量100μL,分离和测定三甲基硒离子、硒代蛋氨酸、亚硒酸和硒酸盐只需8min。HPLC-FAAS在线分析4种硒化合物的检测限为p(Se)=1mg/L。用超声雾化器作ICP-MS的接口,HPLC-ICP-MS在线分析4种硒化合物的检测限分别为P(Se)=0.34μg/L(亚硒酸),0.18μg/L(硒代蛋氨酸),0.08μg/L(三甲基硒离子)和0.07μg/L(硒酸盐)。与气动雾化器接口相比,信号强度增加7至31倍。
A speciation method was developed for selenious acid, selenic acid, trimethylselenonium ion (TMSe)and selenomethionine (SeMet). Separation of the four selenium species was achieved by HPLC on an ESA Anion Ⅲanion-exchange column using aqueous mobile phase of 5. 5 mmol/L ammonium citrate at pH 5. 5 with a flow rate of 1. 5 mL/min. Under the optimal conditions, the four selenium species were separated within 8 minutes. On-line selenium--specific detection was carried out with an inductively coupled plasma mass spectrometer (ICP-MS) or a flame atomic absorption spectrometer (FAAS). The detection limits of HPLC-FAAS were approximately p(Se)=1 mg/L for each compound (100 μL injection). To increase the nebulization efficiency of the ICP-MS, the Meinhard concentric nebulizer was replaced by an ultrasonic nebulizer (USN). The ICP-MS signal intensity was increased by a factor of 7 for selenious acid and 24 to 31 for TMSe, SeMet and selenic acid with the USN compared to that with the Meinhard nebulizer. The detection limits of the HPLC-USN-ICP-MS were p(Se)=0. 08 μg/L for TMSe, p(Se)=0. 34 μg/L for selenious acid, p(Se) = 0. 18 μg/L for SeMet and p(Se) =0. 07 μg/L for selenic acid.
出处
《色谱》
CAS
CSCD
北大核心
1999年第3期240-244,共5页
Chinese Journal of Chromatography
关键词
HPLC
ICP
MS
FAAS
测定
硒化合物
high performance liquid chromatography, inductively coupled plasma-mass spectrometer, flame atomic absorption spectrometer, selenium compound, speciation