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  

Determination of total aluminum in wheat by ultra wave digestion-inductively coupled plasma optical emission spectrometry

作　　者：卢丽[1,2] 刘二龙 詹业添[1,2] 谢湘娜 王岚[1,2] 李波平 刘艳艳[1,2] 覃小燕 邹志飞[1,2] 

机构地区：[1]广东检验检疫技术中心,广州510623 [2]广东省动植物与食品进出口技术措施研究重点实验室,广州510623 [3]黄埔出入境检验检疫局,广州510730

出　　处：《食品安全质量检测学报》2018年第3期564-569,共6页Journal of Food Safety and Quality

基　　金：广东出入境检验检疫局科技计划项目(2017GDK47);食品安全国家标准(spaq-2016-153);"十三五"国家重点研发计划(2017YFF0211300)~~

摘　　要：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（HNO_3-H_2O_2 digestive system, HNO_3-HF-H_2O_2 digestive system, HNO_3-HF-HCL digestive system） and ultra wave digestion method（HNO_3-HF-H_2O_2 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（HNO_3-HF-H_2O_2 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（HNO_3-HF-H_2O_2 system）, and it＇s more accurate and can be used for the determination of total aluminum in wheat samples.

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 

分 类 号：O657.31[理学—分析化学] TS210.7[理学—化学]