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目的建立微波消解-电感耦合等离子质谱法(microwave digestion-inductively coupled plasma mass spectrometry,MWD-ICP-MS)同时测定蜂胶中铅(Pb)、砷(As)、汞(Hg)、镉(Cd)、铬(Cr)5种常见重金属元素。方法样品加HNO_3 5.0 m L和H_2O_2 1.0 m L进行微波消解,赶酸温度为110℃;采用ICP-MS法直接测定Pb、As、Hg、Cd、Cr 5种重金属元素的含量。结果 Pb、As、Cd、Cr在1~500μg/L线性范围内,Hg在1~5.0μg/L线性范围内都具有良好的线性关系,相关系数r>0.999,检出限为0.012~0.015 mg/kg,加标回收率为95.3%~101.8%。该方法测得蜂胶中的Pb含量为2.16 mg/kg、As含量为0.23 mg/kg、Hg含量为0.03 mg/kg、Cd含量为0.06 mg/kg、Cr含量为1.2 mg/kg。结论该方法具有良好的准确度和精密度,检出限低,适用于蜂胶中常见重金属元素的同时测定。
Objective To establish a microwave digestion-inductively coupled plasma mass spectrometry (MWD-ICP-MS) system for the simultaneous determination of lead, arsenic, mercury and cadmium in propolis, Chromium (Cr) 5 kinds of common heavy metal elements. The samples were subjected to microwave digestion with HNO3 5.0 m L and H202 1.0 m L, and the hops temperature was 110 ℃. The contents of Pb, As, Hg, Cd and Cr were determined directly by ICP-MS. Results Pb, As, Cd and Cr were linear in the range of 1 ~ 500 μg / L. Hg showed good linearity in the linear range of 1 ~ 5.0 μg / L with the correlation coefficient of r> 0.999 and the detection limit of 0.012 ~ 0.015 mg / kg, the recoveries were 95.3% ~ 101.8%. The results showed that Pb content in propolis was 2.16 mg / kg, As content was 0.23 mg / kg, Hg content was 0.03 mg / kg, Cd content was 0.06 mg / kg and Cr content was 1.2 mg / kg. Conclusion The method has good accuracy and precision, low detection limit, and is suitable for the simultaneous determination of common heavy metal elements in propolis.