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| ICP-MS和原子荧光光谱测定油脂中总砷的关键点控制和差异性研究 |
| Key point of control and differences of determination of total arsenic in edible oil by ICP-MS and atomic fluorescence spectrometry |
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| DOI： |
| 中文关键词: 总砷 油脂 微波消解 电感耦合等离子质谱法 原子荧光光谱法 |
| 英文关键词:total arsenic oil microwave digestion inductively coupled plasma mass spectrometer atomic fluorescence spectroscopy |
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| 中文摘要: |
| 研究了电感耦合等离子质谱仪（ICP-MS）和原子荧光光度计（AFS）两种检测方法测定油脂中总砷的关键点控制和差异性。对葵花籽油、大豆油、油茶籽油、玉米油、花生油5种油脂及其加标样品进行微波消解，并分别采用ICP-MS和AFS法测定样品中总砷的含量。结果表明：选择国产UP级硝酸，控制赶酸温度140?℃，赶酸余量0.5 mL，赶酸时间2 h左右，以及AFS法检测时加入10%100 g/L硫脲+抗坏血酸溶液延长反应时间至1 h，可以保证检测结果的准确性和重现性；ICP-MS和AFS法加标回收率分别为97.7%~104.2%、92.6%~1050%。研究发现优化后的两种方法检测油脂中总砷含量无显著性差异。 |
| 英文摘要: |
| The key point of control and differences of determination of total arsenic in edible oil by inductively coupled plasma mass spectrometer(ICP-MS) and atomic fluorescence spectrometry(AFS) were studied. Sunflower seed oil, soybean oil, oil-tea camellia seed oil, corn oil, peanut oil and standard-added samples were digested by microwave, and the total arsenic content in the samples were determined by ICP-MS and AFS. The results showed that domestic nitric acid of level UP, controling acid evaporation temperature 140?℃, acid evaporation residual amount 0.5 mL, acid evaporation time around 2 h, 100 g/L thiourea + ascorbic acid solution dosage 10%, and reaction time 1 h in AFS detection were selected, which could guarantee the accuracy of test results and repeatability. The recovery rates of ICP-MS and AFS were 97.7%-104.2% and 92.6%-105.0%, respectively. In addition, it was found that there was no significant difference in the total arsenic content determination by the two methods. |
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