高效液相色谱-电感耦合等离子体质谱法测定鱼肉中的3种汞形态

Detection of mercury speciation in fish by HPLC coupled with ICP-MS

目的利用高效液相色谱与电感耦合等离子体质谱联用技术的高灵敏度和低检出限,建立鱼肉中3种汞形态的高效液相色谱(HPLC)-电感耦合等离子体质谱(ICP-MS)法。方法样品用25%四甲基氢氧化铵溶液微波提取法,流动相定容,C18反相色谱柱分离,电感耦合等离子体质谱检测。结果在600 s内可成功分离3种形态的汞化合物,甲基汞(Me Hg+)、无机汞(Hg2+)和乙基汞(Et Hg+)的浓度为0.05μg/L^1.00μg/L时,线性关系良好,相关系数(r)≥0.999 7,方法的检出限为0.002 5μg/L^0.005 0μg/L。在低、中、高3种浓度下,方法回收率为93.0%~103.3%。结论该方法操作简便、实用性强、结果可靠,可以用于鱼肉中低含量汞形态的检测。

Objective Using high sensitivity and low detection limits of high performance liquid chromatography（ HPLC） coupled with inductively coupled plasma mass spectrometry（ ICP- MS）,to develop a simple method for the determination of three mercury species in fish by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry（ HPLC- ICP- MS）. Methods The mercury species in sample were microwave assisted extracted with 25% tetramethylammonium hydroxide as extract solvent,with the mobile phase for quantification,when the chromatographic separation was performed on C18 column and detected with inductively coupled plasma mass spectrometry. Results Within 600 s,three mercury species（ inorganic mercury,methylmercury and ethylmercury） were separated. The limits of detection（ LODs） were among0. 002 5 μg / L- 0. 005 0 μg / L,good linearity was obtained when the concentration was among 0. 05 μg / L- 1. 00 μg / L,with the correlation coefficient greater than 0. 999 7. The recoveries of the method in low,medium and high concentrations were among 93. 0%- 103. 3%. Conclusion The method is simple,practical,reliable,and it is suitable for the determination of low content mercury species in fish.