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快速自动的方法,无需外部预处理,通过氢化物发生和原子荧光光谱检测直接测定葡萄汁样品中的总锑。

Fast automated method for the direct determination of total antimony in grape juice samples by hydride generation and atomic fluorescence spectrometric detection without external pretreatment.

机构信息

Universidade Federal da Paraíba, Departamento de Química, P.O. Box 5093, Zip Code 58051-970, João Pessoa, PB, Brazil.

Universidade Federal de Alagoas, Instituto de Química e Biotecnologia, Campus A.C. Simões, Tabuleiro dos Martins, 57072-900, Maceió, AL, Brazil.

出版信息

Food Chem. 2022 Jul 1;381:132194. doi: 10.1016/j.foodchem.2022.132194. Epub 2022 Jan 21.

Abstract

Matrix complexity of fruit juices and their low antimony level requires sensitive, cost-effective instruments, time-consuming and error-prone sample pretreatment methods. Therefore, a flow-batch procedure (HG-FBA-AFS) was developed for the fast and sensitive determination of total inorganic Sb in grape juice samples by hydride generation atomic fluorescence spectrometry. The sample pretreatment, pre-reduction and stibine formation steps run through the mixing chamber. The HCl and NaBH concentrations, and carrier gas flowrate were optimized through a Box-Behnken design. The detection limit (LOD) was 20 ng L, intra and inter-day precision ranged in 3.0 - 3.5 %, and low errors within (- 2.4 to 6.6 %) for samples containing 1.23 - 4.58 µg L total Sb. Both HG-FBA-AFS and reference method agreed at 95% confidence level. An 87 h sample throughput, and a 1.15 mL total waste per determination attest that HG-FBA-AFS is a fast, and ecofriendly tool for determining Sb in grape juices.

摘要

果汁基质复杂且锑含量低,这就要求使用灵敏、经济高效的仪器和耗时且易出错的样品预处理方法。因此,本文建立了一种流动进样-批次处理(HG-FBA-AFS)程序,通过氢化物发生原子荧光光谱法快速、灵敏地测定葡萄汁样品中的总无机锑。样品的预处理、预还原和生成氢化物步骤在混合室内完成。通过 Box-Behnken 设计对 HCl 和 NaBH₄浓度以及载气流速进行了优化。检测限(LOD)为 20ng/L,对于含 1.23-4.58μg/L 总锑的样品,日内和日间精密度在 3.0-3.5%之间,误差较低(-2.4 至 6.6%)。HG-FBA-AFS 和参考方法在 95%置信水平下一致。HG-FBA-AFS 每批测定的样品通量为 87h,总废物量为 1.15mL,表明该方法是一种快速、环保的测定葡萄汁中锑的工具。

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Effect of sample preparation procedure for the determination of As, Sb and Se in fruit juices by HG-ICP-OES.
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