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Optimization of the operating conditions of solid sampling electrothermal vaporization coupled to inductively coupled plasma optical emission spectrometry for the sensitive direct analysis of powdered rice

机译:固体采样电热汽化与电感耦合等离子体发射光谱法联用的米粉直接分析的优化

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摘要

Two different approaches were used to improve the capabilities of solid sampling (SS) electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP-OES) for the direct analysis of powdered rice. Firstly, a cooling step immediately before and after the vaporization step in the ETV temperature program resulted in a much sharper analyte signal peak. Secondly, point-by-point internal standardization with an Ar emission line significantly improved the linearity of calibration curves obtained with an increasing amount of rice flour certified reference material (CRM). Under the optimized conditions, detection limits ranged from 0.01 to 6 ng g~(-1) in the solid, depending on the element and wavelength selected. The method was validated through the quantitative analysis of corn bran and wheat flour CRMs. Application of the method to the multi-elemental analysis of 4-mg aliquots of real organic long grain rice (white and brown) also gave results for Al, As, Co, Cu, Fe, Mg, Se, Pb and Zn in agreement with those obtained by inductively coupled plasma mass spectrometry following acid digestion of 0.2-g aliquots. As the analysis takes roughly 5 min per sample (2.5 min for grinding, 0.5-1 min for weighing a 4-mg aliquot and 87 s for the ETV program), this approach shows great promise for fast screening of food samples.
机译:两种不同的方法用于提高固体采样(SS)电热汽化(ETV)与电感耦合等离子体发射光谱(ICP-OES)耦合的能力,以直接分析大米粉。首先,在ETV温度程序中,在蒸发步骤之前和之后的冷却步骤会导致更尖锐的分析物信号峰。其次,使用Ar发射线进行的逐点内部标准化显着改善了用增加的米粉认证参考材料(CRM)所获得的校准曲线的线性。在最佳条件下,固体中的检出限范围为0.01到6 ng g〜(-1),这取决于所选的元素和波长。通过对玉米麸和小麦粉CRM的定量分析验证了该方法的有效性。该方法在真正的有机长粒大米(白色和棕色)的4毫克等分试样的多元素分析中的应用也得出了Al,As,Co,Cu,Fe,Mg,Se,Pb和Zn的结果,与酸消解0.2 g等分试样后,通过电感耦合等离子体质谱法获得的样品。由于每个样品的分析大约需要5分钟(研磨需要2.5分钟,称量4毫克等分试样需要0.5-1分钟,ETV程序需要87 s),因此这种方法显示了快速筛选食品样品的巨大希望。

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