Zhongguo youzhi (Feb 2022)
电感耦合等离子体质谱法测定蛋黄卵磷脂中15种金属元素Determination of 15 kinds of metal elements in egg yolk lecithin by inductively coupled plasma mass spectrometry
Abstract
蛋黄卵磷脂样品经微波消解，采用电感耦合等离子体质谱法测定样品中15种金属元素含量，对检测条件进行了优化，并进行了方法学考察。结果表明，在射频功率1.55 kW、载气（高纯氩气）流速 1.03 L/min、等离子气体流速15.0 L/min、蠕动泵转速 0.1 r/s、采样深度 10 mm、重复次数 3 次条件下，通过在线加入内标钪(Sc)、锗(Ge)、铟(In)、铼(Re)元素可校正基体效应和干扰，测定汞元素时，加入金元素可降低测定误差；该方法的15 种金属元素线性关系良好，线性相关系数（R）均大于0.999；方法检出限在0.03～0.65 ng/mL之间，定量限在0.10～1.97 ng/mL之间；仪器精密度良好，RSD在0.45%～4.67%之间；重复性RSD在1.78%～8.72%之间；中间精密度RSD在2.24%～9.45%之间；加标回收率在92.67%～132.90%之间, RSD在1.42%～7.00%之间。样品溶液在2~8 ℃条件下保存72 h，稳定性良好，RSD在0.56%～3.93%之间。该方法快速、准确、灵敏度高, 可用于蛋黄卵磷脂中15种金属元素的同时测定。 Egg yolk lecithin samples were digested by microwave and 15 kinds of metal elements in it were determined by inductively coupled plasma mass spectrometry(ICP-MS). The detection conditions were optimized and the methodology was investigated. The results showed that under the conditions of RF power 1.55 kW, flow rate of carrier gas(high purity argon)1.03 L/min, flow rate of plasma gas 15.0 L/min, peristaltic pump speed 0.1 r/s, sampling depth 10 mm and 3 replications, the internal standard solution with Sc，Ge，In and Re were added online for matrix effect and interference correction, and Au was added when determining the content of Hg to reduce the test error. The linearities for the 15 elements of the method were good with the correlation coefficients（R）above 0.999. The detection limit and quantitation limit of 15 elements were 0.03-0.65 ng/mL and 0.10-1.97 ng/mL, respectively. The precisions of the instrument were good with RSD in the range of 0.45%-4.67%. The RSD of the repeatability test was in the range of 1.78%-8.72%.The RSD of the intermediate precision was in the range of 2.24%-9.45%. The recovery rate of the 15 elements was in the range of 92.67%-132.90% with RSD in the range of 1.42%-7.00%. The stability of the sample solution was good and when it was stored at 2-8 ℃ for 72 h, RSD was in the range of 0.56%-3.93%. The method had advantages of fastness, accuracy and high sensitiveness, and it could be used for simultaneous determination of 15 kinds of metal elements in egg yolk lecithin.
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