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中国精品科技期刊2020
秦慧芳,王颖,彭俏,等. 微波消解-火焰原子吸收光谱法测定油脂样品中的9种金属元素[J]. 食品工业科技,2022,43(11):334−341. doi: 10.13386/j.issn1002-0306.2021100066.
引用本文: 秦慧芳,王颖,彭俏,等. 微波消解-火焰原子吸收光谱法测定油脂样品中的9种金属元素[J]. 食品工业科技,2022,43(11):334−341. doi: 10.13386/j.issn1002-0306.2021100066.
QIN Huifang, WANG Ying, PENG Qiao, et al. Determination of Nine Metal Elements in Oil Samples by Flame Atomic Absorption Spectrometry with Microwave Digestion[J]. Science and Technology of Food Industry, 2022, 43(11): 334−341. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021100066.
Citation: QIN Huifang, WANG Ying, PENG Qiao, et al. Determination of Nine Metal Elements in Oil Samples by Flame Atomic Absorption Spectrometry with Microwave Digestion[J]. Science and Technology of Food Industry, 2022, 43(11): 334−341. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021100066.

微波消解-火焰原子吸收光谱法测定油脂样品中的9种金属元素

Determination of Nine Metal Elements in Oil Samples by Flame Atomic Absorption Spectrometry with Microwave Digestion

  • 摘要: 为建立一种能对油脂样品中9种金属元素含量进行准确测定的方法,以5种食用油和2种地沟油为试材,采用微波消解法对样品进行前处理,利用火焰原子吸收光谱仪进行测定,并对微波消解油脂样品时的程序和条件进行了设计和优化,最终建立了包含5个步骤的微波消解新程序,其中最大消解压力为35 atm,最大温度为190 ℃,保持时间为20 min。方法性能考察表明:9种待测金属元素在各自的浓度范围内均具有良好的线性关系,决定系数为0.9982~0.9994,检出限为0.0013~0.0122 μg/mL,样品的加标回收率范围在98.94%~101.45%之间,RSD≤4%(n=6)。采用所建方法对7种油脂样品中的9种金属元素进行了含量测定,检测结果表明:5种食用油中含有丰富的营养元素,而Cr、Cd、Pb元素未检出,初步判断油脂的营养价值和安全性较高。而地沟油样品由于检出含有Cr、Cd、Pb,且Pb的含量远超国家标准限定值,已不适宜食用。实际应用表明:所建方法具有操作简便、准确度高等优点,能满足各类油脂中金属元素的检测需要。

     

    Abstract: To establish an accurate determination method of metal elements in oils, 5 edible oils and 2 gutter oils were chose as raw material, and a new microwave digestion method was established to pretreat oils in this paper. The contents of metals were determined by flame atomic absorption spectrometry. The programs and conditions of microwave digestion were designed and optimized, and finally a new program for microwave digestion containing 5 steps was obtained, which was with a maximum digestion pressure of 35 atm, a maximum temperature of 190 ℃ and a retention time of 20 min. The performances of the established method were investigated and listed as follows: The linear relations of 9 metal elements were good in their concentration ranges, the determination coefficient ranged was from 0.9982 to 0.9994, the limits of detection was ranged from 0.0013 to 0.0122 μg/mL, and the standard recoveries of samples were ranged from 98.94% to 101.45%, RSD≤4% (n=6). The contents of 9 metal elements in 7 oil samples were determined using this method. The results showed that the nutritional elements in 5 edible oils were rich, and the contents of Cr , Cd and Pb were not detected, therefore, estimated preliminary, the nutritional value and safety of the oils were high. However, Cr, Cd and Pb in gutter oils were all detected, and the contents of Pb are far higher than the threshold limit value of national standard, so the gutter oils are not suitable for consumption. These applications showed that the method has many advantages of simple operation and high accuracy, the needs of determination of metal elements in oils can be satisfied.

     

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