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目的建立电感耦合等离子体质谱法(ICP-MS)测定样品中汞的方法。方法样品经微波消解处理,加入L-半胱氨酸(0.1%)和金(200μg/L),使其形成金汞齐和较稳定的络合物,减少容器对其吸附作用及记忆效应,用电感耦合等离子体质谱仪进行测定。结果通过对各类标准物质及样品的检测,线性方程为y=2.568×10-3x+3.34×10-4,相关系数(r)为0.999 9。食品样品按0.5 g取样量计算方法的检出限为11μg/kg。以精密度考察方法重现性,相对标准偏差(RSD)均<5.0%,加标回收考察方法准确性,加标回收率为97.5%~102.5%。方法的各指标结果均令人满意。结论本方法操作简便快捷,线性范围宽,灵敏度高,准确可靠,很好的解决了汞的吸附问题和记忆效应,用无碰撞池的电感耦合等离子体质谱仪测汞,能得到满意的结果。
Objective To establish a method for the determination of mercury in samples by inductively coupled plasma mass spectrometry (ICP-MS). Methods The samples were treated with microwave digestion, adding L-cysteine (0.1%) and gold (200μg / L) to form gold amalgam and more stable complexes to reduce the adsorption effect and memory effect of the container. Inductively coupled plasma mass spectrometry was used for the determination. The results of various types of reference material and sample testing, the linear equation was y = 2.568 × 10-3x + 3.34 × 10-4, the correlation coefficient (r) was 0.999 9. The detection limit of the food sample according to 0.5 g sampling method is 11 μg / kg. The repeatability of the method was investigated by precision. The relative standard deviations (RSDs) were all less than 5.0%. The accuracy of the spiked method was tested by spike recoveries. The recoveries were 97.5% -102.5%. The results of the method are satisfactory. Conclusions The method is simple, rapid, linear range, high sensitivity, accurate and reliable. It solves the problem of mercury adsorption and memory effectively, and can obtain satisfactory results with mercury in the collision-free pool ICP-MS.