为全面明确农产品中各种微量元素的分布,确保农产品的质量安全控制,利用多模式进样系统和电感耦合等离子体发射光谱分析技术,提出了同时测定糙米中氢化物发生元素(As、Se、Sn、Sb、Hg)和非氢化物发生元素(Cr、Mn、Fe、Ni、Cu、Zn、Mo、Sr、Cd、Pb)的新策略。采用微波消解系统消解糙米样品,在MSIS的双重模式下利用ICP-OES对样品消解溶液中的多种微量元素进行测定。通过在线加入20 g/L L-半胱氨酸/40 g/L 酒石酸的混合溶液为预还原剂提高氢化物发生元素的发生效率,根据光谱响应数据解卷积构建快速自动曲线拟合技术(fast automatic curve fitting technology, FACT)模型校正光谱重叠和背景干扰,采用Y和Bi为内标元素校正基体效应,使用国家标准参考物质湖南大米(GBW10045)评价分析方法的准确可靠性。结果表明,各元素仪器的检出限为0.01~1.06 μg/L,平均加标回收率为93.0%~106%,相对标准偏差为2.2%~4.9%。所建立的方法适用于糙米中多元素的高通量分析。
To comprehensively clarify the distribution of the trace elements in agricultural products and ensure the quality and safety control of agricultural products, a multimode sample introduction system (MSIS) and inductively coupled plasma optical emission spectrometry (ICP-OES) were used. A new strategy for simultaneous determination of hydride-generation elements (As, Se, Sn, Sb, Hg) and non-hydride-generation elements (Cr, Mn, Fe, Ni, Cu, Zn, Mo, Sr, Cd, Pb) in brown rice was proposed. The brown rice samples were digested by a microwave digestion system. The MSIS was operated in dual mode and the multi-elements in the sample solution were determined by ICP-OES. The efficiency of hydride-generation elements was improved by adding a mixed solution of 20 g/L L-cysteine/40 g/L tartaric acid online as a pre-reducing agent, and the fast automatic curve fitting technology (FACT) model was constructed based on the deconvolution of the spectral response data to correct for spectral overlap and background interference. Y and Bi were selected as the internal standard element to correct the matrix effect, and the national standard reference material Hunan rice (GBW10045) was used to evaluate the accuracy and reliability of the analytical method. Results showed that the limit of detection (LOD) was 0.01-1.06 μg/L, the spiked recovery was 93.0%-106%, and the relative standard deviation was 2.2%-4.9%. The developed method is suitable for high-throughput analysis of multi-elements in brown rice.
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