高效液相色谱-原子荧光光谱法测定水产品中 不同形态汞含量

Determination the content of mercury in different speciations in aquatic products by high performance liquid chromatography-atomic fluorescence spectrometry

中文关键词:  高效液相色谱-原子荧光光谱法  高效液相色谱-电感耦合等离子体质谱法  无机汞  甲基汞  乙基汞  水产品

英文关键词:high efficiency liquid chromatography-atomic fluorescence spectroscopy  high efficiency liquid chromatography-inductively coupled plasma-mass spectrometry  inorganic mercury  methylmercury  ethyl mercury  aquatic products

中文摘要:

      目的 建立高效液相色谱-原子荧光光谱法(high efficiency liquid chromatography-atomic fluorescence spectroscopy, HPLC-AFS)测定水产品中不同形态汞的含量, 并以高效液相色谱-电感耦合等离子体质谱法(high efficiency liquid chromatography-inductively coupled plasma-mass spectrometry, HPLC-ICP-MS)进行方法确证。方法 样品中的汞元素经5 mol/L HCl溶液提取, 用6 mol/L NaOH溶液中和样品, L-半胱氨酸作为流动相中的汞配位剂, 用于样品中不同形态汞的分离。结果 汞化合物在质量浓度为1.0~20.0 μg/L范围内, 浓度和光谱峰面积间呈良好的线性关系。方法检出限分别为: 无机汞0.009 mg/kg、甲基汞0.006 mg/kg和乙基汞0.009 mg/kg; 加标回收率为81.0%~117.0%, 相对标准偏差为3.59%~7.30%。用本方法对FAPAS质控样品蟹肉罐头T07231QC中的甲基汞进行测定, 测定的结果值与参考值相符。结论 该方法操作简单、灵敏度高、重现性好, 适用于水产品中不同形态汞含量的测定及结果确证。

英文摘要:

      Objective To establish A method for to determination the content of mercury in different speciations in aquatic products by high performance liquid chromatography-atomic fluorescence spectrometry and to confirm this method by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry. Methods The mercury element in samples were extracted by 5 mol/L HCl solution, 6 mol/L NaOH solution was used to neutralize the sample, and L-cysteine was used as mercury complexing agent in mobile phase. Results The mercury compounds showed a good linear relationship between concentration and peak area in the range of 1.0~20.0 g/L. The detection limits of quantification of inorganic mercury, methylmercury and ethylmercury were 0.009 mg/kg, 0.006 mg/kg and 0.009 mg/kg, respectively. Recoveries and relative standard deviations were 81.0%~117.0% and 3.59%~7.30%, respectively. The method was used to determine the methyl mercury in canned of FAPAS T07231QC sample, and the measured results were in good agreement with the reference values. Conclusion This method is simple, sensitive and reproducible, and it can be used for the determination of mercury in aquatic products.