基于微波消解的ICP-OES/ICP-MS法测定鸡内金中24种元素

目的：建立电感耦合等离子体发射光谱（ICP-OES）-电感耦合等离子体质谱（ICP-MS）测定鸡内金中24种元素的方法。方法：取样品，加入硝酸8 mL和30%过氧化氢2 mL，经预消解，置微波消解仪中经升温消解、冷却、赶酸至液体剩余约1 mL，将试样溶液转移至50 mL塑料量瓶中，用水稀释至刻度，选择合适的分析谱线和观测方式，以ICP-OES（射频功率1.15 kW，载气流量12 L·min^-1，雾化器压力0.23 MPa，冲洗泵速50 r·min^-1，分析泵速50 r·min^-1；积分时间：短波长15 s，长波长5 s；样品冲洗时间30 s）测定了鸡内金中Na（钠）、Mg（镁）、P（磷）、S（硫）、K（钾）和Ca（钙）；通过选择合适的同位素，以Sc（钪）、Ge（锗）、In（铟）、Bi（铋）为内标溶液消除基体干扰，ICP-MS用KED模式（碰撞反应池技术）测定了Li（锂）、Al（铝）、V（钒）、Cr（铬）、Mn（，锰）、Fe（铁）、Co（钴）、Ni（镍）、Cu（铜）、Zn（锌）、As（砷）、Rb（铷）、Sr（锶）、Mo（钼）、Cd（镉）、Ba（钡）、Hg（汞）和Pb（铅）。结果：各元素的线性良好，相关系数R²>0.999，ICP-OES和ICP-MS检出限分别在0.74~10.26 μg·L^-1和0.002~0.098 μg·L^-1之间，方法精密度（RSD）在1.8%~8.4%范围内。利用本方法测定了鸡肉国家标准物质（GBW10018），测定值与标准值基本相符。样品测定结果表明：鸡内金中含量较高的元素有Na、Mg、P、S、K、Ca、Al、Mn、Fe、Cu和Zn等。结论：本方法适用于鸡内金等动物类中药中多元素的同时测定。

Objective: To establish a method based on inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) for determination of 24 elements in chicken gizzard membrane. Methods: ICP-OES was applied to determine the elements of Na, Mg, P, S, K and Ca by choosing suitable analytical spectral lines and observation mode, the elements (Li, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Rb, Sr, Mo, Cd, Ba, Hg and Pb) were determined by ICP-MS, and the matrix effect and the mass spectrum interferences were corrected by selecting the appropriate isotopes, using internal standards (Sc, Ge, In, Bi) and KED mode (collision reaction cell technology). Results: Linear correlation coefficients of these elements were better than 0.999. The limits of detection of ICP-OES and ICP-MS were in the range of 0.74-10.26 μg·L^-1 and 0.002-0.098 μg·L^-1, respectively. The precision for this method varied from 1.8% to 8.4%. The established method was applied to determine the certified reference materials of chicken (GBW10018), giving results in consistency with the certified values. The results showed that there were rich Na, Mg, P, S, K, Ca, Al, Mn, Fe, Cu and Zn in chicken gizzard membrane. Conclusion: The method is suitable for the determination of multi-elements in traditional Chinese medicine based on animal origin, such as chicken gizzard membrane.