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    盐酸超声提取-高分辨电感耦合等离子体质谱法测定食用植物油中11种微量金属元素

    Determination of 11 Trace Metel Elements in Edible Vegetable Oil by High-Resolution Inductively Coupled Plasma Mass Spectrometry after Ultrasonic Extraction with Hydrochloric Acid

    • 摘要: 提出了盐酸超声提取-高分辨电感耦合等离子体质谱法(HR-ICP-MS)快速测定食用植物油中铝、钡、镉、铜、铁、镁、锰、镍、铅、钒、锌等微量金属元素的方法。取2.0 g食用植物油样品,置于50 mL塑料离心管中,加入800 μL ICP溶剂油,于旋涡混匀器上充分混匀,加入10 mL 2.0 mol·L−1盐酸溶液,于70 ℃超声30 min,冷却。以转速10 000 r·min−1离心5 min,在水相与有机相分离后,收集水相,采用HR-ICP-MS测定其中11种元素含量,待测同位素51V、56Fe、27Al、63Cu、24Mg、55Mn、60Ni、66Zn选择中分辨率模式,而137Ba、111Cd和208Pb选择低分辨率模式。结果表明:11种元素的质量浓度在100 μg·L−1以内与对应的信号强度呈线性关系,检出限(3s)为0.012~0.173 μg·L−1;按照标准加入法对食用植物油进行回收试验,回收率为86.9%~107%,测定值的相对标准偏差(n=7)为1.1%~4.9%;方法用于分析3种植物油样品,本方法测定值与标准方法的测定值基本一致。

       

      Abstract: A method for the rapid determination of trace metel elements including aluminum, barium, cadmium, copper, iron, magnesium, manganese, nickel, lead, vanadium, and zinc in edible vegetable oil by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) after ultrasonic extraction with hydrochloric acid was proposed. 2.0 g of edible vegetable oil sample was taken into a 50 mL-plastic centrifuge tube, and 800 μL of ICP solvent oil was added. After thoroughly mixing on a vortex mixer, 10 mL of 2.0 mol·L−1 hydrochloric acid solution was added, and the mixture was sonicated at 70 ℃ for 30 min and cooled. The mixture was centrifuged at a rotational speed of 10 000 r·min−1 for 5 min. After separating the aqueous phase from the organic phase, the aqueous phase was collected, in which 11 elements were determined by HR-ICP-MS, with medium resolution mode for isotopes to be tested of 51V, 56Fe, 27Al, 63Cu, 24Mg, 55Mn, 60Ni, and 66Zn, and low resolution mode for 137Ba, 111Cd, and 208Pb. As shown by the results, linear relationships between the corresponding response intensity and mass concentrations of 11 elements were found within 100 μg·L−1, with detection limits (3s) of 0.012—0.173 μg·L−1. Test for recovery was made on edible vegetable oil sample by standard addition method, giving results in the range of 86.9%—107%. RSDs (n=7) of the determined results were in the range of 1.1%—4.9%. The method was applied to analysis of 3 edible vegetable oil samples, and the determined values of this method were basically consistent with those of the standard methods.

       

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