Sugaring-out assisted extraction (SoAE): A novel approach for the determination of Cd and Pb in milk by graphite furnace atomic absorption Spectrometry

IF 5.7 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta Pub Date : 2025-06-20 DOI:10.1016/j.aca.2025.344347

Eduardoda Silva G. de Castro , Ricardo J. Cassella

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引用次数: 0

Abstract

Background

Milk and dairy products are significant from both nutritional and economic perspectives. As a result, they are subject to strict health surveillance and quality control protocols, making the development of reliable analytical methods a critical concern in the food industry. Due to the complex and variable chemical composition of milk matrix, sample preparation steps are often essential prior to the determination of metals using spectroanalytical techniques.

Results

This study introduces a novel sample preparation method for the determination of Cd(II) and Pb(II) in milk, based on extraction assisted by the sugaring-out effect (SoAE), using acetonitrile as the extraction solvent. Quantification of the analytes in the extracts was carried out using Graphite Furnace Atomic Absorption Spectrometry (GF AAS). The optimized method achieved limits of quantification (LoQs) of 0.24 μg kg⁻¹ for Cd(II) and 1.3 μg kg⁻¹ for Pb(II), with enhancement factors of 7.5 and 9, respectively. These LoQs are well below the maximum allowable limits for these contaminants in milk (50 μg kg⁻¹ for Cd(II) and 10 μg kg⁻¹ for Pb(II)), confirming the suitability of the method for routine quality control. The method was rigorously validated in accordance with requirements set by international regulatory bodies. Its accuracy, evaluated using a certified reference material (CRM), was 106 % for Cd(II) and 91.8 % for Pb(II).

Significance

The proposed method is novel, using the sugaring-out effect (SoAE) for the first time in metal determination of complex aqueous samples. It offers simplicity, speed, and accurate Cd(II) and Pb(II) determination without interferences. The SoAE approach shows promise for broader applications, including the separation and determination of other metals or organics in combination with various spectroscopic, chromatographic, and electroanalytical techniques.

Abstract Image

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糖化辅助萃取：石墨炉原子吸收光谱法测定牛奶中Cd和Pb的新方法

从营养和经济的角度来看，牛奶和乳制品都很重要。因此，它们受到严格的健康监测和质量控制协议的约束，这使得开发可靠的分析方法成为食品工业的一个关键问题。由于牛奶基质的化学成分复杂多变，在使用光谱分析技术测定金属之前，样品制备步骤通常是必不可少的。结果介绍了一种以乙腈为萃取溶剂，基于糖化萃取（SoAE）辅助萃取法测定牛奶中Cd（II）和Pb（II）的新制样方法。采用石墨炉原子吸收光谱法（GF AAS）对提取物中的分析物进行定量分析。优化后的方法Cd（II）的定量限为0.24 μg kg-1, Pb（II）的定量限为1.3 μg kg-1，增强因子分别为7.5和9。这些loq远低于牛奶中这些污染物的最大允许限值（Cd（II）为50 μg kg-1， Pb（II）为10 μg kg-1），证实了该方法用于常规质量控制的适用性。该方法按照国际监管机构的要求进行了严格的验证。使用认证标准物质（CRM）对其准确度进行评估，Cd（II）的准确度为106%，Pb（II）的准确度为91.8%。意义本方法新颖，首次将糖化效应（SoAE）用于络合水样中金属的测定。它提供了简单，快速和准确的Cd（II）和Pb（II）的测定无干扰。SoAE方法显示出更广泛的应用前景，包括与各种光谱、色谱和电分析技术相结合的其他金属或有机物的分离和测定。

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来源期刊

Analytica Chimica Acta 化学-分析化学

CiteScore

10.40

自引率

6.50%

发文量

1081

审稿时长

38 days

期刊介绍： Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review. Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.