微波消解电感耦合等离子体质谱法同时测定大黄鱼中12种无机元素含量

    Simultaneous Determination of 12 Inorganic Elements in Pseudosciaena Crocea by Microwave Digestion and Inductively Coupled Plasma Mass Spectrometry

    • 摘要: 采用HNO3-H2O2酸消解体系对大黄鱼样品进行微波消解前处理,电感耦合等离子体质谱仪同时测定大黄鱼中Mg、Ca、Fe、Cu、Zn、Se、Mn、Sr、Pb、Cr、Hg、Cd等12种无机元素含量。通过对电感耦合等离子体质谱仪器条件进行优化、选取合适的同位素、应用动能歧视模式克服质谱干扰,在线加入内标校正基体效应并补偿信号漂移,标准曲线法进行定量分析。结果表明:12种无机元素在一定的浓度范围内有良好的线性关系,相关系数r均大于0.999,加标回收率为88.0%~102.0%,相对标准偏差RSD≤5.9%,选用国家标准物质大虾(GBW10050)为质控样验证方法准确性,12种无机元素含量的测定值均落在证书值参考范围内。该方法具有检测快捷简便、检出限低、线性范围宽、准确度和精密度高、回收率好、可多元素同时测定的优点,能满足大批量的大黄鱼中多种无机元素含量的测定分析要求。

       

      Abstract: The samples of Pseudosciaena crocea were digested by using HNO3-H2O2 acid digestion system before microwave digestion. The contents of 12 inorganic elements including Mg, Ca, Fe, Cu, Zn, Se, Mn, Sr, Pb, Cr, Hg and Cd in Pseudosciaena crocea were simultaneously determined by inductively coupled plasma mass spectrometry. By optimizing the instrument conditions of inductively coupled plasma mass spectrometer, selecting suitable isotopes and applying the model of kinetic energy discrimination to overcome the interference of mass spectrometry, the internal standard was added online to correct the matrix effect and compensate the signal drift, and the quantitative analysis was carried out by using the standard curve method. The results showed that there was a good linear relationship among the 12 inorganic elements within a certain concentration range, and the correlation coefficient r was greater than 0.999, the recovery rates were 88.0%-102.0%, and the relative standard deviation (RSD) was less than 5.9%. The accuracy of the method was verified by using the national standard material prawn (GBW10050) as the quality control sample, and the determination values of 12 inorganic elements all fell within the reference range of the certificate values. This method had the advantages of quick and simple detection, low detection limit, wide linear range, high accuracy and precision, good recovery rate, and the simultaneous determination of multi-elements, which could meet the requirements for the determination and analysis of multiple inorganic elements in large quantities of Pseudosciaena crocea.

       

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