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电感耦合等离子体发射光谱法测定高油脂和非油脂类植物中钾和磷样品前处理方法研究

Pretreatment Method for Determination of Kalium and Phosphorus in High Oil and Grease and Non-oil Plant Samples by Inductively Coupled Plasma-Optical Emission Spectrometry

  • 摘要: 测定植物样品中的钾和磷,通常采用高压密闭微波消解-电感耦合等离子体发射光谱法(ICP-OES),但复杂的基质会增加消解难度,如花生、核桃等含有高油脂类大分子聚合物的样品难以快速消解彻底,易使测定结果偏低。为了提高植物中钾和磷的检测效率,本文采用硫酸-过氧化氢消解法和高压密闭微波消解处理样品,将待测元素磷转化成磷酸盐,钾成为游离的钾离子,形成单相单价态消解溶液,通过对比实验确定了应用ICP-OES快速、准确测定不同类型样品中钾和磷含量的前处理方法。经实际样品分析验证表明:①对于高油脂类样品,硫酸-过氧化氢消解法通过强酸破坏植物外层结构,使有机物快速炭化,随后滴加过氧化氢快速消解(约2.5h),能直接消解样品,且消解更安全和彻底;而高压密闭微波消解法耗时较长(约4.5h);与大多学者研究结果对比,硫酸-过氧化氢消解法准确度优于高压密闭微波消解法,建议优先采用。②对于非油脂类样品,2种处理方式均适宜,钾和磷测定结果无显著性差异,并且与目前大多学者的研究结果较为一致,其中高压密闭微波消解法试剂消耗少、空白值低、操作简便,建议优先采用。③硫酸-过氧化氢消解法测定钾和磷的方法检出限分别为0.006mg/L和0.001mg/L,对于高油脂类样品RSD在1.32%~1.98%之间,相对误差在-0.007%~-0.025%之间,重复性r在2.92%~8.21%之间;对于非油脂类样品RSD在0.51%~0.87%之间,相对误差在-0.002%~0.010%之间,重复性r在0.770%~5.08%之间;高压密闭微波消解法测定钾和磷的方法检出限分别为0.005mg/L和0.001mg/L,对于高油脂类样品中钾和磷的相对误差在-0.012%~-0.028%之间,非油脂类样品中钾和磷的相对误差在-0.010%~0.001%之间。④硫酸-过氧化氢消解法能够快速消解高油脂类植物样品,但湿法消解仍然受样品性质的复杂程度以及消解的外部环境等因素影响。

     

    Abstract:
    BACKGROUND The determination of kalium and phosphorus in plant samples is usually carried out by high-pressure sealed microwave digestion-inductively coupled plasma-optical emission spectrometry (ICP-OES).However, complex matrices can increase the difficulty of digestion, such as peanuts, walnuts, and other samples containing high oil and grease macromolecular polymers, which are difficult to digest quickly and thoroughly, easily leading to low results.
    OBJECTIVES To improve the efficiency for the determination of kalium and phosphorus in plants.
    METHODS Sulphuric acid-hydrogen peroxide digestion and high pressure sealed microwave digestion were used to convert the elemental phosphorus into phosphate and the kalium into free potassium ions to form a single-phase monovalent digestion solution.
    RESULTS Validation of the actual sample analysis showed that: (1) For high oil and grease samples, the sulphuric acid-hydrogen peroxide digestion method can directly digest the sample by destroying the outer layer structure of the plant by strong acid, causing rapid charring of the organic matter, followed by rapid digestion (about 2.5h) by dropwise addition of hydrogen peroxide, which is safer and more thorough; whereas the high-pressure sealed microwave digestion method is more time-consuming (about 4.5h).Compared with the results of most scholars, the sulphuric acid-hydrogen peroxide method is recommended, because its accuracy is better than that of the high-pressure sealed microwave method.(2) For non-oil samples, both treatments are suitable and there is no significant difference between the results of kalium and phosphorus determination, with the high-pressure sealed microwave digestion method being recommended for its low reagent consumption, low blank value and ease of operation.The results of the two methods are in good agreement with the experimental results of most scholars.(3) The limits of detection for kalium and phosphorus by the sulfuric acid-hydrogen peroxide digestion method were 0.006mg/L and 0.001mg/L, respectively.For the high oil and grease samples, the RSD ranged from 1.32% to 1.98%, the repeatability r ranged from 2.90% to 8.21% and the error of determination ranged from-0.007% to-0.025%.For the non-oil samples, the RSD ranged from 0.51% to 0.87%, the repeatability r ranged from 0.77% to 5.08%, and the error of determination ranged from-0.002% to 0.010%.The limits of detection for kalium and phosphorus by high pressure sealed microwave digestion were 0.005mg/L and 0.001mg/L, respectively.For the high oil and grease samples, the error of determination for kalium and phosphorus ranged from-0.012% to-0.028%;for the non-oil samples, and the error of determination for kalium and phosphorus ranged from-0.010% to 0.001%.
    CONCLUSIONS The sulphuric acid-hydrogen peroxide digestion method is capable of rapidly digesting high oil and grease macromolecular polymers, but it is affected by the complexity of the samples and the external environment.With the development of science and technology, direct solid injection with artificial intelligence will be the future trend.

     

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