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中国精品科技期刊2020
熊善波,何鲒,张阔,等. HPLC-ICP-MS结合微波酸提取分析测定干制食用菌中砷的形态[J]. 食品工业科技,2021,42(10):236−241. doi: 10.13386/j.issn1002-0306.2020060175.
引用本文: 熊善波,何鲒,张阔,等. HPLC-ICP-MS结合微波酸提取分析测定干制食用菌中砷的形态[J]. 食品工业科技,2021,42(10):236−241. doi: 10.13386/j.issn1002-0306.2020060175.
XIONG Shanbo, HE Jie, ZHANG Kuo, et al. Determination of Arsenic Species in Dried Edible Fungi by HPLC-ICP-MS Combined with Microwave Acid Extraction Analysis [J]. Science and Technology of Food Industry, 2021, 42(10): 236−241. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020060175.
Citation: XIONG Shanbo, HE Jie, ZHANG Kuo, et al. Determination of Arsenic Species in Dried Edible Fungi by HPLC-ICP-MS Combined with Microwave Acid Extraction Analysis [J]. Science and Technology of Food Industry, 2021, 42(10): 236−241. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020060175.

HPLC-ICP-MS结合微波酸提取分析测定干制食用菌中砷的形态

Determination of Arsenic Species in Dried Edible Fungi by HPLC-ICP-MS Combined with Microwave Acid Extraction Analysis

  • 摘要: 本文将微波酸提取与高效液相色谱-电感耦合等离子体质谱法联用技术相结合,建立了一种简单、高效的分析方法用于检测干制食用菌中砷的形态化合物。通过对提取方式比较和提取条件的优化,进而验证方法的精密度、检出限、准确度和加标回收率。结果表明:采用微波酸提取方式,既能满足提取效率,又能保证了各砷形态之间不发生转变。在10 min内实现亚砷酸根(As(Ⅲ))、砷酸根 (As(V))、一甲基砷(MMA)、二甲基砷 (DMA)、砷甜菜碱(AsB)、砷胆碱(AsC)的分离。线性关系良好(r>0.9990) ,相对标准偏差(RSD%)<10.0%,定量限分别为0.009、0.012、0.013、0.010、0.011、0.010 mg/kg。以羊肚菌、黑松露两种基质进行加标回收实验,回收率在83.6~105.5%之间;采用两种标准物质验证了方法的准确性好。本方法前处理简单、分离效果、精密度好、准确度高,适用于干制食用菌中砷形态的分析测定,为扩容国标方法适用范围提供了一种新的检测方法和推动食用菌无机砷限量值的制定提供基础数据。

     

    Abstract: In this paper, microwave acid extraction and HPLC-ICP-MS were combined to establish a simple and efficient method for the determination of arsenic speciation in dried edible fungi. By comparing the extraction methods and optimizing the extraction conditions, the precision, detection limit, accuracy and recovery of the method were verified. The results showed that the microwave-acid extraction method not only satisfied the extraction efficiency, but also ensured that the forms of arsenic did not change. The separation of (As (III), As (V), MMA, DMA, ASB, ASC was realized within 10 minutes. The linear relationship was good (r > 0.9990), RSD%<10.0%. The quantitative limits were 0.009, 0.012, 0.013, 0.010, 0.011 and 0.010 mg/kg, respectively. The recoveries of morels and black truffle were 83.6%~105.5%. The accuracy of the method was verified by two kinds of standard materials. The method had the advantages of simple pretreatment, good separation effect, good precision and high accuracy, and was suitable for the analysis and determination of arsenic species in dried edible fungi, and it would provide a new method for the determination of inorganic arsenic in edible fungi and basic data for the determination of inorganic arsenic limit in edible fungi.

     

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