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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 Na OH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1.0~20.0μg/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。
OBJECTIVE To establish a method for the determination of mercury in aquatic products by high-performance liquid chromatography-atomic fluorescence spectroscopy (HPLC-AFS). The contents of mercury in different forms of aquatic products were determined by high performance liquid chromatography-inductively coupled plasma mass spectrometry efficiency liquid chromatography-inductively coupled plasma-mass spectrometry, HPLC-ICP-MS). Methods The mercury in the sample was extracted with 5 mol / L HCl solution, the sample was neutralized with 6 mol / L NaOH solution and L-cysteine was used as the Hg complexing agent in the mobile phase for different forms of mercury The separation. Results The concentration of mercury compounds in the range of 1.0 ~ 20.0 μg / L showed a good linear relationship between the peak area and the concentration of mercury compounds. The detection limits were as follows: inorganic mercury 0.009 mg / kg, methylmercury 0.006 mg / kg and ethyl mercury 0.009 mg / kg; the recoveries were 81.0% ~ 117.0% with relative standard deviations of 3.59% -7.30% . The method was used to determine the methylmercury in the TAP7231QC sample of Crab meat from FAPAS quality control sample. The measured value was consistent with the reference value. Conclusion The method is simple, sensitive and reproducible. It is suitable for the determination of mercury in different forms of aquatic products and the confirmation of results.