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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Enzyme-assisted extraction and liquid chromatography-inductively coupled plasma mass spectrometry for the determination of arsenic species in fish
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Enzyme-assisted extraction and liquid chromatography-inductively coupled plasma mass spectrometry for the determination of arsenic species in fish

机译:酶辅助提取和液相色谱 - 电感耦合等离子体质谱法测定鱼类中砷物种

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摘要

A sensitive, simple and rapid method for the simultaneous determination of eleven arsenic species has been developed. A high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) technique was used for the analysis of eleven arsenic species in less than 17 min. Different extraction solutions were explored and the recovery results using water and aqueous acidic solvents, aqueous organic solvents and enzymes showed that 40 mg protease with 0.75 mL 0.5% hydrochloric acid (v/v) as the extraction agent gave the best experimental results. Species separation with ammonium carbonate solution as the mobile phase was conducted on an anion-exchange chromatographic column using gradient elution. The column temperature was 20 degrees C and kinetic energy discrimination (KED) was employed to eliminate spectral interference. The use of KED mode effectively removed interference from (ArCl)-Ar-75. The detection limit (L-D) of the method was in the range of 0.11-0.59 mu g kg(-1). Repeatability values obtained for spiked real fish samples were in the range of 1.1%-7.6%. Accuracy was calculated based on the analysis of spiked real fish samples at five concentration levels. Obtained recoveries were 91%-106%. The validated method was used in a pilot study to analyze real samples of fish, the organic arsenic especially AsB was the major arsenic specie present in the analyzed samples, only trace amount of inorganic arsenic were detected. The analytical method should improve the assessment of human exposure associated with arsenic intake from fish. (C) 2018 Elsevier B.V. All rights reserved.
机译:已经开发出一种敏感,简单,快速的同时测定11砷物种的方法。高效液相色谱 - 电感耦合等离子体质谱(HPLC-ICP-MS)技术用于分析在不到17分钟的少于17分钟内的11种。探索不同的提取溶液,使用水和酸性溶剂,水性有机溶剂和酶的回收结果表明,40mg蛋白酶,0.75ml 0.5%盐酸(v / v),因为萃取剂得到了最佳的实验结果。使用梯度洗脱在阴离子交换色谱柱上进行与碳酸铵溶液的物种分离。柱温为20℃,采用动能辨别(KED)来消除光谱干扰。 kEd模式的使用有效地从(ARCL)-AR-75中干扰。该方法的检测限(L-D)为0.11-0.59μgkg(-1)。用于尖刺的真实鱼样品获得的可重复性值在1.1%-7.6%的范围内。基于在五个浓度水平的尖刺真实鱼类样品的分析来计算精度。获得的回收率为91%-106%。验证的方法用于试验研究以分析鱼类的真正样品,有机砷特别是ASB是分析的样品中存在的主要砷物种,仅检测到痕量的无机砷。分析方法应改善与鱼类砷摄入相关的人体暴露的评估。 (c)2018年elestvier b.v.保留所有权利。

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