HPLC-ICP-MS法测定水产动物及其制品中5种砷形态的含量
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(1. 漯河出入境检验检疫局,河南 漯河 462000;2. 启迪桑德环境资源股份有限公司,北京 101102)

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王林裴(1989—),女,漯河出入境检验检疫局助理工程师,硕士。E-mail:13839513071@163.com

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Determination of five arsenic species in aquatic animals and their products by high performance liquid chromatography and inductively coupled plasma mass spectrometry
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(1. Luohe Entry-Exit Inspection and Quarantine Bureau of P.R.C, Luohe, Henan 462000, China; 2. Beijing Sound environment Group Ltd., Beijing 101102, China)

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    摘要:

    建立了高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用法测定水产动物及其制品中的砷酸根\[As(Ⅴ)\]、亚砷酸根\[As(Ⅲ)\]、砷甜菜碱AsB、一甲基砷(MMA)和二甲基砷(DMA)5种形态的砷。用0.15 mol/L的硝酸水溶液作为提取液,样品在80 ℃下微波消解30 min,上清液供HPLC-ICP-MS进行分析。5种砷形态采用Hanmilton PRX-X100(250 mm×4.1 mm,10 μm)阴离子色谱柱分离,经ICP-MS检测。比较了不同的洗脱方式对5种砷形态的分离效果,研究了色谱条件对砷形态的分离度的影响并进行优化。通过加标回收试验考察了方法准确度,在3个加标水平上各形态的回收率为87.8%~97.5%,试验测定得出相对标准偏差(n=6)均<5%,5种砷形态在0~100 μg/L时呈现良好的线性,方法检出限为0.002~0.010 mg/kg。结果显示,该方法提取简单、灵敏度高、重现性好,可用于水产动物及其制品中砷形态的检测。

    Abstract:

    A method was developed for the simultaneous determination of arsenic acid \[As(Ⅴ)\], arsenious acid \[As(Ⅲ)\], arsenobetaine (AsB), monomethyl arsonic acid (MMA) and dimethylarsinic acid (DMA) in aquatic animals and their products by high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The extraction reagent was 0.15 mol/L nitric acid with heat-assistant condition for 30 min at 80 ℃. Then, the five arsenic species were separated by a anion exchange column (Hanmilton PRX-X100 250 mm×4.1 mm, 10 μm) and detected by ICP-MS. The effects of different elution methods on the separation of five arsenic forms were compared, and the chromatographic conditions on the separation of arsenic were studied and optimized. The recoveries of the five arsenic species spiked in aquatic animals at three levels ranged from 87.8%~97.5%, and the relative standard deviations (n=6) were 1.5%~4.5%. The five arsenic species showed good linearity in the range of 0~100 μg/L, and the limits of detection for the five arsenic species were 0.002~0.010 mg/kg. This method was simple, accurate and durable for the detection of arsenic species in aquatic animals and their products.

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王林裴,郑亚哲,彭新然. HPLC-ICP-MS法测定水产动物及其制品中5种砷形态的含量[J].食品与机械,2017,33(11):61-66.
WANGLinpei, ZHENGYazhe, PENGXinran. Determination of five arsenic species in aquatic animals and their products by high performance liquid chromatography and inductively coupled plasma mass spectrometry[J]. Food & Machinery,2017,33(11):61-66.

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  • 在线发布日期: 2023-03-10
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