摘要
建立了超声酸提取-高效液相-原子荧光联用测定温州海产品中无机汞[Hg(Ⅱ)]、甲基汞(MeHg)和乙基汞(EtHg)含量的方法,并优化了实验条件。实验采用5mol/L盐酸溶液,超声3.0h提取汞化合物,硫代硫酸钠络合,最后经C18柱(4.6mm×150mm)分离,流动相为5%乙腈-0.06mol/L乙酸铵-0.12%L-半胱氨酸。在最佳条件下,3种汞化合物在0—20μg/L范围内线性良好,相关系数(r)均优于0.9990,检出限分别为1.04、1.09和1.29μg/L,相对标准偏差(RSDs)均小于5%(n=10),温州海产品的汞加标回收率达到90.1%—107.3%。该方法操作简便,精密度高,干扰少,适用于各地海产品中汞化合物的形态分析测定。
A ultrasonic extract-HPLC-AFS method was established for determination of mercury speciation,including inorganic mercury [Hg（ 11 ）],methylmercury （MeHg） and etlaylmercury （EtHg） in Wenzhou seafood, and the experiment conditions were optimized, simaltaneously. Three hour ultrasonication assisted 5mol/L HC1 to extract mercury,then chelated with NazS2Os,finally separated on a C18 chromatographic column （4.6mm × 150mm） using 5% acetonitrile-0.06mol/L ammonium acetate-0. 12% L-cysteine as mobile phase. Under the optimized conditions, the linear ranges for Hg（ Ⅱ ）,MeHg, EtHg were between 0--20μg/L,with correlative coefficients more than 0. 9990. The detection limits were 1.04,1.09,1.29lag/L, respectively,and the relative standard deviations （n=10） for the mercury species were all under 5%. The spiked recoveries for mercury compounds in Wenzhou seafood were range from 90.1% to 107.3 %, The proposed method of HPLC-AFS is simple,accurate, no interference,and was suitable for the soeciation of mercnrv in seafnnd.
出处
《光谱实验室》
CAS
2013年第3期1335-1339,共5页
Chinese Journal of Spectroscopy Laboratory
