超级微波消解-电感耦合等离子体发射光谱测定小麦中总铝含量
目的 比较不同前处理消解方法, 建立电感耦合等离子体发射光谱法(inductively coupled plasma optical emission spectrometry, ICP-OES)测定小麦样品中总铝的准确分析方法。方法 采用4种样品前处理方法: 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－盐酸体系)、超级微波消解(硝酸－氢氟酸－双氧水体系), 消化标准参考物质大米(GBW10045)和玉米粉(GBW10012), 采用ICP-OES法测定, 同时用添加回收实验验证方法的准确性与可靠性。结果 采用超级微波消解方法(硝 酸－氢氟酸－双氧水体系)时, 标准参考物质的铝含量测定结果在标准参考值范围内, 采用其他样品前处理方法时的测定结果远低于参考值范围。该方法在0.04~5.0 mg/L浓度范围内线性关系良好, r=0.9999, 方法定量限为2.0 mg/kg, 回收率为91%~118%, 相对标准偏差(relative standard deviation, RSD)为1.4%~4.5%。结论 小麦样品中可能存在铝被硅包裹的现象, 采用硝酸－氢氟酸－双氧水体系超级微波消解方式能将其消解完全, 使检测结果更加准确, 该法可用于小麦样品中总铝的测定。
Objective To compare different sample digestion methods and establish an accurate method for the determination of the total aluminum in wheat samples by inductively coupled plasma optical emission spectrometry (ICP-OES). Methods National standard substance rice powder (GBW10045) and corn powder (GBW10012) were digested by 4 kinds of different sample digestion methods, including microwave digestion method (HNO3-H2O2 digestive system, HNO3-HF-H2O2 digestive system, HNO3-HF-HCL digestive system) and ultra wave digestion method (HNO3-HF-H2O2 digestive system). The aluminum content was determined by ICP-OES. The accuracy and reliability of these methods were verified by recovery tests. Results The determination result of aluminum content in the standard reference material by the ultra wave digestion method (HNO3-HF-H2O2 digestive system) was within the standard reference range, but the results of the other 3 kinds of sample pretreatment methods were far below the reference range. The calibration curve showed good linearity in the range of 0.04~5.0 mg/L with correlation of 0.9999, the limit of quantitation was 2.0 mg/kg, the recovery rate was 91%~118%, and the relative standard deviation (RSD) ranged from 1.4% to 4.5%. Conclusion There may be aluminum which is encapsulated by silicon in wheat samples. The wheat samples can be digested completely under the ultra-wave digestion (HNO3-HF-H2O2 system), and it’s more accurate and can be used for the determination of total aluminum in wheat samples.
标题：超级微波消解-电感耦合等离子体发射光谱测定小麦中总铝含量
英文标题：Determination of total aluminum in wheat by ultra wave digestion-inductively coupled plasma optical emission spectrometry
作者：
卢丽 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
刘二龙 黄埔出入境检验检疫局
詹业添 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
谢湘娜 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
王岚 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
李波平 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
刘艳艳 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
覃小燕 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
邹志飞 广东检验检疫技术中心,广东省动植物与食品进出口技术措施研究重点实验室
中文关键词:超级微波消解,总铝,小麦,电感耦合等离子体发射光谱法,
英文关键词:ultra wave digestion,total aluminum,wheat,inductively coupled plasma optical emission spectrometry,
发表日期：2017-11-10
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