{"title":"超声辅助制样后HPLC - ICP-MS联合测定海产品样品中砷的种类。","authors":"Sabriye Sel, Büşra Aydoğan, İkbal Koyuncu","doi":"10.1016/j.talanta.2025.128518","DOIUrl":null,"url":null,"abstract":"<p><p>In this study, an analytical method was applied for the separation and determination of inorganic and organic arsenic species (As<sup>+3</sup>, As<sup>+5</sup>, AsB, MMA) in anchovy, haddock, mussels and prawns using HPLC coupled with ICP-MS. Efficient separation of the arsenic species on the HPLC-ICP-MS system was achieved using 50 mM (NH<sub>4</sub>)<sub>2</sub>CO<sub>3</sub> at pH 9.50 diluted in 1 % methanol and 0.50 mM EDTA as mobile phase. The arsenic species were extracted from the samples by means of ultrasonically assisted sample preparation. The LOD/LOQ values of the detection system were 0.07/0.22 ng/mL, 0.12/0.41 ng/mL, 0.06/0.22 ng/mL and 0.03/0.11 ng/mL for arsenobetaine (AsB), As<sup>+3</sup>, methylarsonic acid (MMA) and As<sup>+5</sup>, respectively. The relative standard deviations calculated for the lowest calibration standards ranged between 1.01 and 7.88 %, verifying good precision for replicate measurements. The accuracy of the method was validated by spike recovery experiments, with recorded recoveries in the range of 85-117 %.The total arsenic content of the extracts was determined by direct ICP-MS analysis. A certificated reference material (NIST-1573A) was analyzed for the total As concentration. The method was successfully applied for the qualitative and quantitative determination of AsB, As<sup>+3</sup>, MMA and As<sup>+5</sup> in the seafood samples ranging from 6.0 to 5700 ng/g. The carcinogenic and non-carcinogenic risk for haddock and anchovies was low, whereas the carcinogenic risk for prawns was relatively high but below the threshold value, according to the risk assessment of the samples.</p>","PeriodicalId":435,"journal":{"name":"Talanta","volume":"296 ","pages":"128518"},"PeriodicalIF":6.1000,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Determination of arsenic species in seafood samples using a combination of HPLC and ICP-MS after ultrasonic assisted sample preparation.\",\"authors\":\"Sabriye Sel, Büşra Aydoğan, İkbal Koyuncu\",\"doi\":\"10.1016/j.talanta.2025.128518\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>In this study, an analytical method was applied for the separation and determination of inorganic and organic arsenic species (As<sup>+3</sup>, As<sup>+5</sup>, AsB, MMA) in anchovy, haddock, mussels and prawns using HPLC coupled with ICP-MS. 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引用次数: 0
摘要
本文采用HPLC - ICP-MS分离测定了鳀鱼、黑线鳕、贻贝和对虾中无机和有机砷(As+3、As+5、AsB、MMA)的含量。采用50 mM (NH4)2CO3, pH为9.50,1%甲醇稀释,0.50 mM EDTA为流动相,在HPLC-ICP-MS系统上实现了砷的高效分离。采用超声辅助制样方法提取样品中的砷。检测系统对砷甜菜碱(AsB)、As+3、甲基胂酸(MMA)和As+5的LOD/LOQ分别为0.07/0.22 ng/mL、0.12/0.41 ng/mL、0.06/0.22 ng/mL和0.03/0.11 ng/mL。最低标准的相对标准偏差在1.01 ~ 7.88%之间,验证了重复测量的良好精度。通过加标回收率实验验证了该方法的准确性,加标回收率在85 ~ 117%之间。采用直接电感耦合等离子体质谱法测定提取物中总砷含量。采用标准物质(NIST-1573A)测定总砷浓度。该方法可用于6.0 ~ 5700 ng/g海产品样品中AsB、As+3、MMA和As+5的定性和定量测定。根据样本的风险评估,黑线鳕和凤尾鱼的致癌和非致癌风险较低,对虾的致癌风险相对较高,但低于阈值。
Determination of arsenic species in seafood samples using a combination of HPLC and ICP-MS after ultrasonic assisted sample preparation.
In this study, an analytical method was applied for the separation and determination of inorganic and organic arsenic species (As+3, As+5, AsB, MMA) in anchovy, haddock, mussels and prawns using HPLC coupled with ICP-MS. Efficient separation of the arsenic species on the HPLC-ICP-MS system was achieved using 50 mM (NH4)2CO3 at pH 9.50 diluted in 1 % methanol and 0.50 mM EDTA as mobile phase. The arsenic species were extracted from the samples by means of ultrasonically assisted sample preparation. The LOD/LOQ values of the detection system were 0.07/0.22 ng/mL, 0.12/0.41 ng/mL, 0.06/0.22 ng/mL and 0.03/0.11 ng/mL for arsenobetaine (AsB), As+3, methylarsonic acid (MMA) and As+5, respectively. The relative standard deviations calculated for the lowest calibration standards ranged between 1.01 and 7.88 %, verifying good precision for replicate measurements. The accuracy of the method was validated by spike recovery experiments, with recorded recoveries in the range of 85-117 %.The total arsenic content of the extracts was determined by direct ICP-MS analysis. A certificated reference material (NIST-1573A) was analyzed for the total As concentration. The method was successfully applied for the qualitative and quantitative determination of AsB, As+3, MMA and As+5 in the seafood samples ranging from 6.0 to 5700 ng/g. The carcinogenic and non-carcinogenic risk for haddock and anchovies was low, whereas the carcinogenic risk for prawns was relatively high but below the threshold value, according to the risk assessment of the samples.
期刊介绍:
Talanta provides a forum for the publication of original research papers, short communications, and critical reviews in all branches of pure and applied analytical chemistry. Papers are evaluated based on established guidelines, including the fundamental nature of the study, scientific novelty, substantial improvement or advantage over existing technology or methods, and demonstrated analytical applicability. Original research papers on fundamental studies, and on novel sensor and instrumentation developments, are encouraged. Novel or improved applications in areas such as clinical and biological chemistry, environmental analysis, geochemistry, materials science and engineering, and analytical platforms for omics development are welcome.
Analytical performance of methods should be determined, including interference and matrix effects, and methods should be validated by comparison with a standard method, or analysis of a certified reference material. Simple spiking recoveries may not be sufficient. The developed method should especially comprise information on selectivity, sensitivity, detection limits, accuracy, and reliability. However, applying official validation or robustness studies to a routine method or technique does not necessarily constitute novelty. Proper statistical treatment of the data should be provided. Relevant literature should be cited, including related publications by the authors, and authors should discuss how their proposed methodology compares with previously reported methods.