超声辅助酸提取-液相色谱-电感耦合等离子体质谱法测定鱼肉中3种汞形态

Determination of inorganic mercury,methyl mercury and ethyl mercury in fish samples by liquid chromatogram-inductively coupled plasma mass spectrometry with ultrasound-assisted acid extraction procedure

目的建立鱼肉中3种汞形态的超声辅助酸提取-液相色谱-电感耦合等离子体质谱(LC-ICP-MS)测定法。方法样品采用超声辅助酸提取,考察了不同浓度盐酸的提取效率,优化了色谱分离条件及电感耦合等离子体质谱分析条件。结果测定了鱼肉中3种汞形态,相对标准偏差值(n=7)<5%,加标回收率在82%~99%之间,方法检出限<6.2μg/kg。结论建立的分析方法准确灵敏、简单稳定,适用于鱼肉中痕量汞形态的分析。

Objective To establish a method for the determination of three mercury speciation in fish samples by liquid chromatogram-inductively coupled plasma mass spectrometry（ LC-ICP-MS） with ultrasound-assisted acid extraction procedure. Methods The sample was extracted with acid under ultrasonic condition. The extraction efficiency of different hydrochloric acid concentration was tested and compared. The chromatographic separation conditions and the operation parameters of ICP-MS were optimized. Results The content of three species in fish samples was determined. Relative standard deviations were less than 5%. The recoveries were in the range of 82%-99%. The detection limit was 6. 2 μg/kg. Conclusion The result indicated that the method was accurate,sensitive,simple,stable and was suitable for the determination of trace mercury speciation in fish.