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高效液相色谱-电感耦合等离子体质谱法分析仿刺参中痕量汞的形态。

Speciation Analysis of Trace Mercury in Sea Cucumber Species of Apostichopus japonicus Using High-Performance Liquid Chromatography Conjunction With Inductively Coupled Plasma Mass Spectrometry.

机构信息

College of Traditional Chinese Medicine, Jilin Agricultural University, Changchun, 130118, China.

Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing, 100193, China.

出版信息

Biol Trace Elem Res. 2018 Dec;186(2):554-561. doi: 10.1007/s12011-018-1309-y. Epub 2018 Mar 25.

Abstract

In this paper, a simple and cost-effective method using high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry with a rapid ultrasound-assisted extraction was used for analysis speciation of trace mercury in sea cucumber species of Apostichopus japonicus. The effective separation of inorganic mercury, methylmercury, and ethylmercury was achieved within 10 min using Agilent ZORBAX SB-C analytical and guard columns with an isocratic mobile phase consisting of 8% methanol and 92% HO containing 0.12% L-cysteine (m/v) and 0.01 mol/L ammonium acetate. Mercury species were extracted from A. japonicus samples using a solution containing 2-mercaptoethanol, L-cysteine, and hydrochloric acid and sonicating for 0.5 h. The limits of detection of inorganic mercury, methylmercury, and ethylmercury were 0.12, 0.08, and 0.20 μg/L, and the minimum detectable concentrations (measured at 0.500 g sample volume in 10.00 mL) were 2.4, 1.6, and 4.0 μg/kg, respectively. Analysis of a scallop certified reference material (GBW 10024) revealed accordance between the experimental and certified values. This study provides a reference for the evaluation of mercury speciation in sea cucumber and other seafood.

摘要

本文采用高效液相色谱-电感耦合等离子体质谱联用,结合快速超声辅助提取法,建立了一种简单、经济的方法,用于分析海参中痕量汞的形态。采用 Agilent ZORBAX SB-C 分析柱和保护柱,以 8%甲醇和 92%HO 为等度流动相,其中含有 0.12% L-半胱氨酸(m/v)和 0.01mol/L 乙酸铵,可在 10min 内实现无机汞、甲基汞和乙基汞的有效分离。采用含 2-巯基乙醇、L-半胱氨酸和盐酸的溶液提取 A. japonicus 样品中的汞形态,超声提取 0.5h。无机汞、甲基汞和乙基汞的检出限分别为 0.12、0.08 和 0.20μg/L,最低检测浓度(以 0.500g 样品体积在 10.00mL 中测量)分别为 2.4、1.6 和 4.0μg/kg。对扇贝标准物质(GBW 10024)的分析表明,实验值与证书值相符。本研究为海参及其他海产品中汞形态的评价提供了参考。

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