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中国无机分析化学:2025,15(3):323-329
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微波消解 - 同位素稀 释- 电感耦合等离子体 质谱(ID - ICP - MS)法测定紫菜中镉
蔡玮1, 张世龙2, 赵博1, 陈欢欢1, 逯海1, 李潇1
(1.中国计量科学研究院;2.江西省检验检测认证总院东华计量测试研究院)
Determination of Cadmium in Laver by Isotope Dilution-Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion
cai wei1, zhang shilong2, zhao bo1, chen huanhuan1, lu hai1, li xiao1
(1.National Institute of Metrology;2.JiangXi General Institute of Testing and Certification Donghua Institute of Metrology and Testing)
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投稿时间:2024-09-29    修订日期:2024-10-28
中文摘要: 紫菜产品中镉污染超标的报道屡见不鲜,准确高效测定紫菜中的镉含量意义重大。建立了一种微波消解-同位素稀释电感耦合等离子体质谱( isotope dilution inductively coupled plasma mass spectrometry,ID-ICP-MS)法对紫菜中镉定量分析的方法,探讨了硝酸、硝酸+过氧化氢、硝酸+氢氟酸三种体系对测定结果的影响,进一步对硝酸+氢氟酸体系中氢氟酸的加入时间及加入量进行优化,并以GBW08521标准物质对方法进行验证。结果表明,硝酸+氢氟酸体系处理紫菜样品的消解效果最佳,氢氟酸宜在消解前加入,且对于0.2 g的紫菜样品,氢氟酸的添加量为0.5 mL即能使其消解完全。与常规ICP-MS定量方法比,ID-ICP-MS法能有效排除基体效应的影响,测量准确度、精密度良好。ID-ICP-MS法测定GBW08521标准物质的镉含量为5.3 mg/kg,扩展不确定度U=0.1 mg/kg,k=2,与标准值相比,归一化偏差|En|=0.25<1,方法准确可靠。此外,加标回收实验中,不同样品的镉加标回收率均在90%~110%,回收效果好。紫菜实际样品分析结果表明,硝酸+氢氟酸消解体系联合ID-ICP-MS法比国标方法GB 5009.268-2016更具普适性。该方法可作为标准物质中镉含量的定值方法,应用于紫菜等复杂基体中镉含量的高精度分析。
Abstract:Its often seen the reports of excessive cadmium (Cd) pollution in laver products, so the accurate and efficient determination of Cd content in laver is of great significance. A method of isotope dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) with microwave digestion was established for the quantitative analysis of Cd in laver. The effects of three digestion systems (includes HNO3, HNO3+H2O2 and HNO3+HF) on the determination results were discussed. The addition time of HF and amount of HF in the HNO3+HF system were further optimized. And the method was verified using Certified Reference Material (GBW08521). The results showed that the HNO3+HF system had the best digestion effect on laver samples, and HF should be added before digestion. What’s more, for 0.2 g amount of laver samples, the addition of 0.5 mL HF can completely digest them. Compared with conventional ICP-MS method, the ID-ICP-MS method can effectively eliminate the influence of matrix effect. And the measurement accuracy and precision of the method are good. The determination of Cd content in GBW08521 reference material by ID-ICP-MS method was 5.3 mg/kg, and the expended uncertainty was 0.1 mg/kg with the coverage factor k=2. Compared with the standard value, the normalized deviation |En| value was 0.25 (smaller than 1), indicating that the method is accurate and reliable. In addition, in the spiked recovery experiment, the Cd spiked recovery rates of different samples were all between 90% and 110%, indicating good recovery effects. The analysis results of actual samples of laver showed that the combination of HNO3+HF digestion system and ID-ICP-MS method is more universal than the national standard method mentioned in GB 5009.268-2016. This method can be used as the determination method of Cd content in reference materials, and can be applied to high-precision analysis of Cd content in complex matrices such as laver.
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基金项目:国家重点研发计划项目(2016YFF0201106),中国计量科学研究院基本科研业务费(AKYZZ2429)
引用文本:
蔡玮,张世龙,赵博,陈欢欢,逯海,李潇.微波消解 - 同位素稀 释- 电感耦合等离子体 质谱(ID - ICP - MS)法测定紫菜中镉[J].中国无机分析化学,2025,15(3):323-329.
cai wei,zhang shilong,zhao bo,chen huanhuan,lu hai,li xiao.Determination of Cadmium in Laver by Isotope Dilution-Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2025,15(3):323-329.

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