稀硝酸-过氧化氢微波消解-电感耦合等离子体发射光谱法测定植物中8种矿物质元素

Determination of 8 Mineral Elements in Plants by Inductively Coupled Plasma-Optical Emission Spectrometry after Microwave Digestion with Dilute Nitric Acid-Hydrogen Peroxide

  • 摘要: 植物作为“土壤-植物-食物链”中矿物质元素循环的关键载体,其体内矿物质元素含量对农产品营养价值评估、食品安全保障等具有重要意义。植物样品有机质含量高、组分复杂,存在基体干扰。样品前处理采用湿法消解易产生有毒气体,干法消解则易造成部分化合物以挥发性物质逸出,影响检测结果准确性。本文在湿法消解基础上进行优化,建立了一种稀硝酸-过氧化氢微波消解电感耦合等离子体发射光谱法(ICP-OES)测定植物样品中Al、Ca、Cu、Fe、K、Mg、Mn、Zn等8种矿物质元素的方法,同时引入相对碳浓度(RCC)小于13%作为消解效率的评价指标。采用“单因素筛选-响应面法”考察了硝酸浓度、消解时间、过氧化氢用量等样品处理条件。在硝酸浓度3.5 mol/L用量5 mL、消解时间15 min、过氧化氢用量2.5 mL条件下,相对碳浓度均小于13%,样品中纤维素、木质素等有机质分解完全。标准物质中Al、Ca、Cu、Fe、K、Mg、Mn、Zn的测定值与标准值基本一致,检出限分别为0.75、1.33、0.12、0.14、0.67、2.12、0.14、0.22 μg/g,准确度(RE)小于12%,相对标准偏差(RSD)小于10%,满足《生态地球化学评价样品分析技术要求(试行)》(DD2005-03)的规定,与文献方法ICP-OES、ICP-MS检测结果的差异不显著。通过实际样品验证,该方法通过RCC指标实现了消解效果的可量化评价,减少试剂用量与环境污染,为元素测定提供了可借鉴的前处理思路。

     

    Abstract: As a key carrier in the mineral element cycle within the “soil-plant-food chain”, the mineral element content in plants is of great significance for the evaluation of agricultural product nutritional value and the assurance of food safety. However, plant samples are characterized by high organic matter content and complex components, which lead to matrix interference. For sample pretreatment, wet digestion is prone to generating toxic gases, while dry digestion tends to cause some compounds to escape as volatile substances—both issues affect the accuracy of detection results. Based on the optimization of wet digestion, this study established a method for determining 8 mineral elements (Al, Ca, Cu, Fe, K, Mg, Mn, and Zn) in plant samples using microwave digestion with dilute nitric acid-hydrogen peroxide combined with inductively coupled plasma-optical emission spectrometry (ICP-OES). Meanwhile, a relative carbon concentration (RCC) of less than 13% was introduced as an indicator to evaluate digestion efficiency. The “single-factor screening-response surface methodology” was adopted to investigate sample treatment conditions such as nitric acid concentration, digestion time, and hydrogen peroxide dosage. Under the optimal conditions (nitric acid concentration of 3.5 mol/L with a volume of 5 mL, digestion time of 15 min, and hydrogen peroxide dosage of 2.5 mL), the RCC was consistently less than 13%, and organic substances such as cellulose and lignin in the samples were completely decomposed. The determined values of Al, Ca, Cu, Fe, K, Mg, Mn, and Zn in the certified reference materials were basically consistent with the standard values. The limits of detection (LOD) for these elements were 0.75, 1.33, 0.12, 0.14, 0.67, 2.12, 0.14, and 0.22 μg/g, respectively. The accuracy (relative error, RE) was less than 12%, and the relative standard deviation (RSD) was less than 10%, which meets the requirements specified in Technical Requirements for Sample Analysis in Eco-Geochemical Evaluation (Trial) (DD2005-03). There was no significant difference between the detection results of this method and those of ICP-OES and ICP-MS methods reported in the literature. Verified by actual samples, this method enables the quantifiable evaluation of digestion efficiency through the RCC index, reduces reagent consumption and environmental pollution, and provides a referable pretreatment approach for element determination.

     

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