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通过对氧化剂的选择、硝酸浓度影响实验和基体改进剂的选择等方面的研究优化了实验条件,最终确定使用硝酸双氧水体系作为氧化剂,选择合适的固液比为:样品/硝酸/过氧化氢=0.25 g/6 m L/2 m L,选择背景较低结果准确可靠的200μg/m L Pd(NO3)2作为基体改进剂,同时选择合适的灰化温度500℃和原子化温度1200℃。对国家标准物质小麦粉进行测定,标准曲线相关系数大于0.999,检出限为0.0003 mg/kg,定量限为0.001 mg/kg,测定结果均在标准值范围内,低含量水平结果RSD为9.1%,高含量水平结果RSD为5.3%。该方法准确可靠、简便安全、总体成本低,尤其适合高通量谷物样品处理。
The experiment conditions were optimized through the selection of oxidant, the influence of nitric acid concentration and the choice of matrix modifier. The final determination of nitric acid hydrogen peroxide system as oxidant and the selection of appropriate solid-liquid ratio were: sample / nitric acid / hydrogen peroxide = 0.25 g / 6 m L / 2 m L, 200 μg / m L Pd (NO 3) 2 was selected as the matrix modifier with lower background accuracy and lower temperature. The suitable ashing temperature was 500 ℃ and the atomization temperature was 1200 ℃. The standard curve of wheat flour was determined. The correlation coefficient of the standard curve was greater than 0.999. The detection limit was 0.0003 mg / kg. The limit of quantification was 0.001 mg / kg. The results were in the standard range. The RSD of low level was 9.1% High level results RSD of 5.3%. The method is accurate and reliable, simple and safe, and low in overall cost, especially for high-throughput cereal sample processing.