微波消解ICP-MS法测定广西北部湾海鸭蛋中硒和锗的含量

以硝酸-过氧化氢（体积比为5：3）混合溶液为消解剂，微波消解法处理海鸭蛋样品，采用电感耦合等离子体质谱法测定样品溶液中的硒和锗的含量。选择适合的同位素元素，运用碰撞室技术（CCT）降低多原子离子对元素硒、锗的干扰，用钇作为在线内标。硒、锗工作曲线的线性范围均为0．0-100．0ng／mL，相关系数r=0．9996；硒、锗的检出限分别为1．1，0．15ng／mL，测定结果的相对标准偏差分别为4．78％，5．70％（n=6），加标回收率为92．2％-104．0％。用该法测定国家标准物质黄鱼（GBW08573）中硒的含量，测定值在标称值范围内。

Determination of Selenium and Germanium in Sea Duck Eggs from Guangxi Beibu Gulf by Microwave Digestion Inductively Coupled Plasma Mass Spectrometry

The sea duck egg sample was dissolved with mixed solution of HNO3-H202 （ volum ratio was 5 ： 3 ） by using microwave digestion, and the Se, Ge in the sample solution were determined by ICP-MS. The appropriate isotopes were selected, the polyatomic ions causing interference were eliminated by collision cell technology（CCT）, and Y was used as internal standard. The liner range of calibration curves for Se and Ge was 0.0-100.0 ng/mL with regression coefficient of 0.999 6. Detection limits of Se andGe were 1.1,0.15 ng/mL respectively, the relative standard deviations of detection results were 4.78%, 5.70%（n=6） respectively, and the recovery ranged from 92.2% to 104%. The method was used in determination of Se in national standard sample （yellow croak GBW08573）, the result was in conformity with standard value.