摘要
目的建立电感耦合等离子体质谱法（ICP-MS）测定谷物样品中铝的准确分析方法。方法本文研究了4种样品前处理方法：干灰化法、微波消解（硝酸-双氧水体系）、微波消解（硝酸-氢氟酸-双氧水体系）、微波消解（硝酸-氢氟酸-双氧水体系消解,加高氯酸二次消解法）,消化大米标准物质（GBW 10010）,采用ICP-MS法测定铝,同时添加回收率来验证不同处理方法的准确性与可靠性。结果对测定结果进行比较分析,前3种消解法的测定值均低于标准值;最后一种消解法在标准值允许范围内;4种前处理方法的检出限在0.42-0.52 mg/kg之间,相对标准偏差3.61%-4.77%（n=6）,加标回收率在92.2%-97.8%之间。结论谷物样品中可能存在酸不溶铝,采取硝酸-氢氟酸-双氧水体系微波消解,加高氯酸二次消解法的方式能将其消解完全,该法可用于谷物样品中铝的测定。
Objective To establish an accurate method for the determination of the aluminum in the grain samples by inductively coupled plasma mass spectrometry（ICP-MS）.Methods Four kinds of different pre-treatment methods were studied,including dry ashing,microwave digestion（HNO3-H2O2 digestive system）,microwave digestion（HNO3-HF-H2O2 digestive system） and microwave digestion（HNO3-HF-H2O2 digestive system,then melted by adding perchloric acid）.National standard substance rice power（GBW 10010） was digested and its aluminum content was determined by ICP-MS.Accuracy and reliability of these methods were verified by recovery test.Results The analysis of the determination showed that the results of these previous 3 kinds of pre-treatment methods were lower than the standard value and the last one was within the standard value.The detection limits of these four kinds of pre-treatment methods varied from 0.42 to 0.52 mg/kg,relative standard deviations（RSDs） varied from 3.61%to 4.77%（n=6） and recoveries were between 92.2%and 97.8%.Conclusion Acid insoluble aluminum exists in the grain samples.Microwave digestion（HNO3-HF-H2O2 digestive system,then melted by adding perchloric acid） can be used in the detection of grain samples as the acid insoluble aluminum can be released through this pre-treatment method.
出处
《食品安全质量检测学报》
CAS
2016年第5期1832-1835,共4页
Journal of Food Safety and Quality
关键词
电感耦合等离子体质谱法
铝
谷物
前处理
inductively coupled plasma mass spectrometry（ICP-MS）
aluminum
grain
pre-treatment methods
