Spectrochimica Acta Part B: Atomic Spectroscopy最新文献_第8页

Early screening of Alzheimer’s disease based on feces analysis using laser-induced breakdown spectroscopy 基于粪便分析的阿尔茨海默病早期筛查，激光诱导击穿光谱

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-22 DOI: 10.1016/j.sab.2025.107372

Wei Cheng , Zhao Zhang , Xueqi Liu , Xiaodong Jin , Yaju Li , Qiang Zeng , Dongbin Qian , Fei Ye , Qiang Li

Alzheimer's disease (AD) poses an unprecedented global health challenge. It exhibits a protracted preclinical phase spanning nearly 20 years, during which early interventions can effectively extend the asymptomatic period, highlighting the critical importance of precision stratification and risk assessment strategies. Current biomarker-based approaches face significant limitations including invasive procedures, high costs, and lack of standardized risk stratification systems, necessitating the development of novel, cost-effective screening technologies for high-risk population identification. In this study, we developed and validated an innovative method using Laser-Induced Breakdown Spectroscopy (LIBS) for screening high-risk populations with preclinical AD characteristics. By analyzing the elemental distribution in feces from 20 AD mice (10 female and 10 male) and 20 age-matched normal mice from 4 to 51 weeks of age, we demonstrated that LIBS can capture subtle changes in metal concentrations associated with AD progression. Principal Component Analysis (PCA) reveals comprehensive alterations in elemental distribution patterns, while a Random Forest (RF) model achieves a classification accuracy exceeding 90 % in most stages. Shapley Additive Explanations (SHAP) analysis identifies Ca II 396.85 nm and Mg 279.55 nm as the most critical spectral features for accurate discrimination, both contributing 14 % to classification accuracy. These findings highlight the potential of LIBS-based fecal analysis as a non-invasive, rapid, and cost-effective tool for early AD screening. This study validated the feasibility of LIBS + machine learning (ML) for screening high-risk AD populations through animal experiments. Nevertheless, extensive studies and technological iterations on the novel LIBS+ML method are required to achieve clinical application standards.

阿尔茨海默病（AD）是一项前所未有的全球健康挑战。它表现出长达近20年的临床前阶段，在此期间早期干预可以有效延长无症状期，突出了精确分层和风险评估策略的重要性。目前基于生物标志物的方法面临着重大的局限性，包括侵入性手术、高成本和缺乏标准化的风险分层系统，因此需要开发新的、具有成本效益的筛查技术来识别高风险人群。在这项研究中，我们开发并验证了一种使用激光诱导击穿光谱（LIBS）筛选具有临床前AD特征的高危人群的创新方法。通过分析20只AD小鼠（10只雌性和10只雄性）和20只年龄匹配的正常小鼠（4至51周龄）粪便中的元素分布，我们证明了LIBS可以捕捉到与AD进展相关的金属浓度的细微变化。主成分分析（PCA）揭示了元素分布格局的全面变化，而随机森林（RF）模型在大多数阶段的分类精度超过90%。Shapley加性解释（SHAP）分析确定Ca II 396.85 nm和Mg 279.55 nm是准确区分的最关键光谱特征，两者都贡献了14%的分类精度。这些发现突出了粪便分析作为一种无创、快速、经济的早期AD筛查工具的潜力。本研究通过动物实验验证了LIBS +机器学习（ML）筛查AD高危人群的可行性。然而，为了达到临床应用标准，需要对新型LIBS+ML方法进行广泛的研究和技术迭代。

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引用次数: 0

Outside Front Cover - Journal name, Cover image, Volume issue details, ISSN, Cover Date, Elsevier Logo and Society Logo if required 外部封面-期刊名称，封面图片，卷刊细节，ISSN，封面日期，爱思唯尔标志和学会标志（如果需要）

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-22 DOI: 10.1016/S0584-8547(25)00248-4

引用次数: 0

Development of a spectral X-ray fluorescence database to strengthen the scientific foundations for the forensic analysis and interpretation of modern soda-lime glass 开发光谱x射线荧光数据库，以加强现代钠钙玻璃的法医分析和解释的科学基础

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-16 DOI: 10.1016/j.sab.2025.107361

Zachary Andrews , Troy Ernst , Cedric Neumann , Tatiana Trejos

This study offers scientific support for the updated standard for micro X-ray fluorescence (μXRF, ASTM E2926) used in forensic glass analysis, reflecting recent changes in modern soda-lime glass formulations and newer μXRF systems with silicon drift detectors (SDDs). To develop this standard, an extensive database has been developed, showing changes in the elemental profiles of modern glass and the forensic implications of the improved analytical capabilities of SDDs. The database comprises over 2000 fragments from 112 known sources of vehicle and architectural windows, including glasses treated with laminating, tempering, and e-coating techniques. The study reveals that different sampling and comparison criteria are required due to the improved precision and sensitivity of SDD and variations in spatial heterogeneity of glass. The comparison interval recommended for older systems with SiLi detectors produces higher false exclusion rates (up to 15 %). Therefore, a modified 3 s comparison criterion is recommended for SDDs to minimize error rates. The modified 3 s criterion accounts for data with precision lower than 3 % RSD by defining the range of the known sample as three times the standard deviation of the measurements or three times 3 % of the mean, whichever is greater. This criterion yielded false exclusion and inclusion rates less than 3 % and 0.7 %, respectively for various sets of full-thickness glass fragments when using at least ten fragments to characterize the heterogeneity of the known sample. The findings raise awareness of the detection of distinctive elements in the nanometer-thick e-coated layer and lead to recommendations for addressing spatial variations.

该研究为法医玻璃分析中使用的微x射线荧光（μXRF, ASTM E2926）的更新标准提供了科学支持，反映了现代钠石灰玻璃配方的最新变化和带有硅漂移检测器（sdd）的新μXRF系统。为了制定这一标准，已经开发了一个广泛的数据库，显示了现代玻璃元素特征的变化以及改进的sdd分析能力的法医意义。该数据库包括来自112个已知来源的车辆和建筑窗户的2000多个碎片，包括经过层压、回火和电子涂层技术处理的玻璃。研究表明，由于SDD的精度和灵敏度的提高以及玻璃的空间异质性的变化，需要不同的采样和比较标准。对于使用SiLi检测器的旧系统，推荐的比较间隔会产生更高的误排除率（高达15%）。因此，建议对sdd使用修改后的3s比较标准，以尽量减少错误率。修正后的3s标准将已知样本的范围定义为测量值的标准偏差的三倍或平均值的三倍，以较大者为准，用于解释精度低于3% RSD的数据。当使用至少10个碎片来表征已知样品的异质性时，该标准产生的假排除率和包含率分别小于3%和0.7%。这些发现提高了人们对纳米厚电子涂层中不同元素检测的认识，并为解决空间差异提出了建议。

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引用次数: 0

Insights into nanoparticle enhanced laser induced breakdown spectroscopy (NELIBS): A comparative study of plasma characteristics and signal enhancement 纳米粒子增强激光诱导击穿光谱（NELIBS）：等离子体特性和信号增强的比较研究

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-16 DOI: 10.1016/j.sab.2025.107358

Morteza Khalaji, Seyed Hassan Tavassoli, Somayeh Karimi

This study investigates the mechanisms behind the spectral emission enhancement in Nanoparticle-Enhanced Laser-Induced Breakdown Spectroscopy (NELIBS) compared to conventional Laser-Induced Breakdown Spectroscopy (LIBS). Using a titanium sample coated with 20 nm spherical Au-NPs under optimized conditions, we analyze the temporal evolution of spectral intensity, plasma properties, and ablation characteristics. The results show that NELIBS sustains higher spectral emission for a longer duration while maintaining a relatively lower plasma temperature and higher electron density during plasma expansion. These conditions promote more efficient recombination processes, enhancing continuum emission. Furthermore, spectral analysis reveals that the NELIBS plasma remains optically thin over an extended time window, contributing to improved signal quality. The primary factor driving this enhancement is the increased density of emitting species (ions and atoms), facilitated by improved laser energy absorption, more efficient plasma formation, and modified ablation mechanisms influenced by the localized surface plasmon resonance (LSPR) effect. Furthermore, the microscopic image confirms that NELIBS results in smoother and more uniform ablation craters, indicating superior ablation efficiency. These insights provide deeper insight into the fundamental differences between LIBS and NELIBS, highlighting the advantages of nanoparticle-assisted plasma generation for enhanced spectroscopic performance.

本研究探讨了纳米粒子增强激光诱导击穿光谱（NELIBS）与传统激光诱导击穿光谱（LIBS）相比，光谱发射增强的机制。在优化条件下，利用包覆20 nm球形Au-NPs的钛样品，分析了光谱强度、等离子体特性和烧蚀特性的时间演变。结果表明，在等离子体膨胀过程中，NELIBS在保持相对较低的等离子体温度和较高的电子密度的同时，在较长的时间内保持较高的光谱发射。这些条件促进了更有效的复合过程，增强了连续体发射。此外，光谱分析表明，NELIBS等离子体在延长的时间窗口内保持光学薄，有助于改善信号质量。驱动这种增强的主要因素是发射物质（离子和原子）密度的增加，促进了激光能量吸收的改善，更有效的等离子体形成，以及局部表面等离子体共振（LSPR）效应影响的改进的烧蚀机制。此外，显微图像证实了NELIBS产生的烧蚀坑更光滑、更均匀，表明了更高的烧蚀效率。这些见解为LIBS和NELIBS之间的根本差异提供了更深入的见解，突出了纳米粒子辅助等离子体生成增强光谱性能的优势。

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引用次数: 0

Determination of the time-evolved electron density and temperature during femtosecond laser filament grooving of silicon carbide ceramic matrix composite 碳化硅陶瓷基复合材料飞秒激光刻丝时电子密度和温度的测定

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-15 DOI: 10.1016/j.sab.2025.107359

Xianwang Li , Tie-Jun Wang , Chaopeng Yang , Xin Gao , Yaoxiang Liu , Yingxia Wei , Hao Qin , Xiangyu Zhang , Jinshan Yang , Zheyuan Hou , Shaoming Dong

The measurements of initial electron temperature and time-evolved electron density are of vital significance in phase change and material removal processes during femtosecond laser fabrication. In this work, two methods were employed to determine the temporal evolution of the electron temperature at different stages during laser filament grooving of the silicon carbide ceramic matrix composite (SiC CMC) by filament-induced breakdown spectroscopy (FIBS), and the time-evolved electron density was determined by the Stark shifting and broadening methods. The initial electron temperature was obtained by fitting the entire temperature evolution using the power-law model after converting the measured temperatures to instantaneous values. The results reveal that, during the early stage, the electron temperatures, derived from the continuum spectrum, undergo a rapid decrease. In contrast, temperature evolution during the later stage, using the Saha-Boltzmann method, shows a slow decay. By applying the power-law fitting and utilizing the measured temperatures, the obtained initial electron temperature was approximately 6.64 eV. The time-evolved electron density measured by the two methods shows consistent results in both magnitude and evolutionary trend. This study not only provides valuable insights into the electron dynamics during ultrafast processing, but also provides key instructions on precisely controlling ultrafast laser processing at the electron level.

在飞秒激光制造过程中，初始电子温度和随时间变化电子密度的测量对相变和材料去除过程具有重要意义。本文采用光纤诱导击穿光谱（FIBS）测定了碳化硅陶瓷基复合材料（SiC CMC）激光开槽过程中不同阶段的电子温度随时间的变化，并采用Stark位移法和展宽法测定了电子密度随时间的变化。将测量温度转换为瞬时值，利用幂律模型拟合整个温度演化过程，得到初始电子温度。结果表明，在初始阶段，由连续谱得出的电子温度急剧下降。与此相反，使用Saha-Boltzmann方法计算的后期温度演变显示出缓慢的衰减。通过幂律拟合并利用实测温度，得到的初始电子温度约为6.64 eV。两种方法测量的随时间变化的电子密度在大小和演化趋势上都显示出一致的结果。该研究不仅为超快加工过程中的电子动力学提供了有价值的见解，而且为在电子水平上精确控制超快激光加工提供了关键指导。

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引用次数: 0

Addition of precipitating element to uniform the distribution of elements in LIBS analysis of liquid samples 在液相色谱分析中加入沉淀元素，使元素分布均匀

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-15 DOI: 10.1016/j.sab.2025.107360

Zhanjian Lin , Lizhu Kang , Wu Wang , Bing Lu , Xiangyou Li

The detection of elements in liquids is one of the core applications of modern analytical chemistry. Laser-induced breakdown spectroscopy (LIBS) shows significant potential for the detection of elements in liquid samples. The dried droplet method (DDM) avoids liquid splashing, but the coffee-ring effect (CRE) in DDM leads to nonuniform distribution of elements, which can reduce the accuracy of quantitative results. In this work, the exogenous precipitating element addition-controlled uniform precipitation (EPEA-CUP) method was proposed to obtain the uniform distribution of the elements. The mechanism by which the addition of precipitated particles suppressed CRE was analyzed. The distribution of the elements was analyzed macroscopically, while their spectral intensities were examined statistically. Based on the distribution of elements, the internal standard method was applied to correct the matrix effect. The R² of Ca, Mg and Na were improved from 0.906, 0.933 and 0.802 to 0.949, 0.982 and 0.997, respectively. This method was used to quantitatively detect Mg, Ca, and Na with high precision and accuracy, which provided an efficient idea for the detection of elements in liquid samples.

液体中元素的检测是现代分析化学的核心应用之一。激光诱导击穿光谱（LIBS）在检测液体样品中的元素方面显示出巨大的潜力。干燥液滴法（DDM）避免了液体的飞溅，但DDM中的咖啡环效应（CRE）导致元素分布不均匀，降低了定量结果的准确性。本文提出了外源沉淀元素添加控制均匀沉淀法（EPEA-CUP）来获得元素的均匀分布。分析了沉淀颗粒的加入抑制CRE的机理。对元素的分布进行了宏观分析，并对其光谱强度进行了统计检验。根据元素的分布情况，采用内标法对矩阵效应进行修正。Ca、Mg和Na的R2分别由0.906、0.933和0.802提高到0.949、0.982和0.997。该方法用于定量检测Mg、Ca、Na，具有较高的精密度和准确度，为液体样品中元素的检测提供了一种高效的思路。

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引用次数: 0

Study on the detection of element content of silicon carbide wafers on different processed surfaces by glow discharge mass spectrometry 辉光放电质谱法检测不同加工表面碳化硅晶圆中元素含量的研究

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-10 DOI: 10.1016/j.sab.2025.107348

Yue Zhang, Xiufang Chen, Xintong Liu, Xiangang Xu, Zhenkai Sun

With the development and application of the third generation of semiconductor materials, impurity analysis of silicon carbide (SiC) wafers has become increasingly crucial. In this study, the glow discharge mass spectrometer (GDMS) was systematically employed to establish the optimal discharge conditions for SiC wafers at 2.5 mA and 1100 V. The relative sensitivity factor (RSF) of aluminum (Al) element was determined and corrected by constructing a calibration curve. The calibration results demonstrated that the RSF value of 1.55 significantly improved the detection accuracy when the Al content ranged from 5 × 10¹⁶ cm⁻³ to 5 × 10¹⁷ cm⁻³. A comprehensive comparative analysis was conducted on wafers subjected to different processing techniques, including wire cutting, grinding, mechanical polishing (MP), and chemical mechanical polishing (CMP). The results demonstrated that wire-cut wafers exhibited markedly elevated surface elemental concentrations compared to other samples. CMP was found to be more effective in reducing the influence of surface impurities on GDMS test results. These results provide valuable insights for optimizing wafer preparation protocols to achieve more accurate impurity characterization in SiC materials.

随着第三代半导体材料的发展和应用，碳化硅（SiC）晶圆的杂质分析变得越来越重要。在本研究中，系统地利用辉光放电质谱仪（GDMS）建立了SiC晶圆在2.5 mA和1100 V下的最佳放电条件。测定了铝元素的相对敏感系数（RSF），并通过建立校准曲线进行了校正。校准结果表明，当Al含量在5 × 1016 cm−3 ~ 5 × 1017 cm−3范围内时，RSF值为1.55显著提高了检测精度。对采用线切割、研磨、机械抛光（MP）和化学机械抛光（CMP）等不同加工工艺的晶圆进行了全面的对比分析。结果表明，与其他样品相比，线切晶片的表面元素浓度明显升高。发现CMP更有效地降低了表面杂质对GDMS测试结果的影响。这些结果为优化晶圆制备方案以实现更准确的SiC材料杂质表征提供了有价值的见解。

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引用次数: 0

Accurate simulation of the CN emission spectra in laser-induced plasma: a joint impact of robust line list, non-LTE conditions and self-absorption effect 激光诱导等离子体中CN发射光谱的精确模拟：鲁棒线表、非lte条件和自吸收效应的共同影响

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-10 DOI: 10.1016/j.sab.2025.107350

Sergey M. Zaytsev, Vera A. Terashkevich

A non-local thermodynamic equilibrium (non-LTE) radiative transfer algorithm, accounting for self-absorption effect explicitly, was implemented for the simulation of high-temperature (T∼4500-6600 K) moderate resolution (Δλ ∼ 0.04 nm) spectra of the diagonal (Δυ=0) bands of B ²Σ⁺ – X ²Σ⁺ (violet) system of the CN radical. The experimental spectra were obtained in laser-induced plasma during the ablation of nitrogen containing carbonaceous solid target in air and emission registration at 12 different delays (0.2-6 μs) after nanosecond laser pulse. A performance comparison of the two publicly available line lists containing spectroscopic data on CN transitions in ExoMol format, namely, Trihybrid and KTPSYT, showed the advantage of the last one for experimental data fitting. Using the KTPSYT line list, a step-by-step expansion of the model was carried out, starting with the single-temperature (T) LTE and optically thin plasma and finishing with the multi-temperature (T_el = T (obtained under LTE condition), T_vib, T_rot) non-LTE optically thick plasma approximations. The multi-temperature Boltzmann distribution of internal kinds of molecular motion was assumed during the non-LTE modeling. The LTE model with self-absorption was applicable for the data explanation obtained at early delays after laser pulse. Both of non-LTE and self-absorption effects appeared at the middle delays and its simultaneous consideration substantially improved the overall fit of the experimental data (the relative squared deviation of the normalized intensity decreased twice down to ∼7 % in comparison with implementation of the simple LTE model without self-absorption). At the late delays the plasma density decreases and the degree of absorption becomes low, whereas the strong difference up to 1800 K is observed between T_vib and T_rot values. The significance of the adjusted plasma parameters was elucidated by routinely errors assessment.

采用一种明确考虑自吸收效应的非局部热力学平衡（非lte）辐射传输算法，对CN自由基B 2Σ+ - X 2Σ+（紫色）体系的对角线（Δυ=0）波段的高温（T ~ 4500 ~ 6600 K）中分辨率（Δλ ~ 0.04 nm）光谱进行了模拟。利用激光诱导等离子体对空气中含氮碳质固体靶进行烧蚀实验，并在纳秒激光脉冲作用下，在12种不同延迟（0.2 ~ 6 μs）下进行发射配准。通过对两种包含ExoMol格式CN跃迁光谱数据的公开线表（即Trihybrid和KTPSYT）的性能比较，发现最后一种线表在实验数据拟合方面具有优势。利用KTPSYT线表，逐步扩展模型，从单温度(T) LTE和光薄等离子体开始，到多温度（Tel = T（在LTE条件下获得），Tvib, Trot）非LTE光厚等离子体近似。在非lte建模过程中，假设内部各种分子运动的多温度玻尔兹曼分布。具有自吸收的LTE模型适用于激光脉冲后早期延迟的数据解释。非LTE和自吸收效应都出现在中间延迟，同时考虑它大大提高了实验数据的整体拟合（与没有自吸收的简单LTE模型的实现相比，归一化强度的相对平方偏差降低了两倍，降至7%）。在延迟后期，等离子体密度降低，吸收程度变低，而Tvib值与Trot值在1800k之前存在较大差异。通过常规误差评估来阐明调整后的血浆参数的意义。

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引用次数: 0

Precision measurement of hyperfine structure of the 2P1/2 and 2P3/2 states in B-like 35,37Cl12+ ions 类b 35,37cl12 +离子中2P1/2和2P3/2态超精细结构的精密测量

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-10 DOI: 10.1016/j.sab.2025.107349

X. Liu , F.H. Qu , W.Q. Wen , X.P. Zhou , A.V. Volotka , Y.S. Kozhedub , D.A. Glazov , D.V. Zinenko , J.G. Li , B. Tu , K. Yao , Y. Yang , B. Wei , X. Ma , Y. Zou , J. Xiao

The hyperfine splitting of highly charged ions has attracted significant interest as a sensitive probe for testing bound-state quantum electrodynamics (QED) and exploring nuclear properties in extreme electromagnetic fields. In this study, we report the first measurement of hyperfine structure in B-like

{Cl}^{12 +}

ions using visible emission spectroscopy with a Czerny–Turner spectrometer at the Shanghai high-temperature superconducting electron beam ion trap (SH-HtscEBIT). Through multi-Gaussian fitting, we extracted the hyperfine structure constants:

A (^{2} P_{1 / 2}) = 36.83 (39)

GHz,

A^{^{'}} (^{2} P_{3 / 2}) = 7.10 (17)

GHz, and

B^{^{'}} (^{2} P_{3 / 2}) = 12.99 (64)

GHz/barn, along with the corresponding fine-structure splitting energies. These results are in good agreement with ab initio QED calculations for

^{35, 37} {Cl}^{12 +}

, and provide direct experimental validation of higher-order interelectronic interaction effects. The present measurement establishes a valuable benchmark for theoretical models of hyperfine structure in mid-

Z

highly charged ions and paves the way for precision tests of bound-state QED in strong-field regimes.

高电荷离子的超细分裂作为一种测试束缚态量子电动力学（QED）和探索极端电磁场下核性质的敏感探针引起了人们的极大兴趣。在这项研究中，我们报道了在上海高温超导电子束离子阱（SH-HtscEBIT）上，首次使用可见光发射光谱测量了类b Cl12+离子的超精细结构。通过多重高斯拟合，我们提取了A(2P1/2)=36.83(39) GHz、A ' (2P3/2)=7.10(17) GHz和B ' (2P3/2)=12.99(64) GHz/barn的超精细结构常数，以及相应的精细结构分裂能。这些结果与35,37cl12 +的从头算QED计算结果很好地吻合，并提供了高阶电子间相互作用效应的直接实验验证。目前的测量为中z高电荷离子的超精细结构理论模型建立了一个有价值的基准，并为强场条件下束缚态QED的精确测试铺平了道路。

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引用次数: 0

Assessment of monochromatic X-ray fluorescence spectrometry as a reliable analytical technique for cadmium quantification in cacao systems 单色x射线荧光光谱法作为可可系统中镉定量可靠分析技术的评价

IF 3.8 2区化学 Q1 SPECTROSCOPY

Spectrochimica Acta Part B: Atomic Spectroscopy

Pub Date : 2025-10-10 DOI: 10.1016/j.sab.2025.107352

Cifuentes MEA , Y. Rodríguez , L.M. Avellaneda-Torres , R. Quiroga-Mateus , D. Bravo

Cadmium in cacao is a key barrier to Colombian exports. Therefore, emergent technologies need to improve Cd testing capacity for cacao. Monochromatic X-ray fluorescence (MXRF) is a cost-effective alternative to conventional techniques such as inductively coupled plasma (ICP-OES/MS) for Cd quantification. MXRF can be applied to solid or liquid samples of cacao farming systems. Although this new technique has demonstrated high accuracy, it has not been validated against major analytical parameters to date. Therefore, the aim of this study was to demonstrate MXRF suitability for cacao and liquid culture samples. The method was validated using soil, soil litter, root, stem, leaf, pod, nib, shell, and Luria-Bertani microbial culture medium. The robustness, limit of quantification (LOQ), trueness, repeatability, intermediate precision, and reproducibility of Cd testing were assessed. Cd correlations between MXRF and ICP was performed using 363 field samples from cacao. The statistical analysis showed a Pearson correlation coefficient between 0.96 and 0.99 and a recovery percentage between 74.8 and 129.9 % for MXRF in comparison to ICP. The robustness parameter identified appropriate laboratory and field pretreatments. Likewise, the choice of measurement time of 60 and 200 s was critical. The LOQ ranged from 0.124 to 0.148 mg kg⁻¹. For the parameter trueness, the % R ranged from 90.7 % to 109.0 %. The Z'-scores for reproducibility ranged from −0.50 to 0.62. The validation demonstrated the suitability of MXRF for Cd testing in cacao systems and liquid media. The impact of this new technology on cacao and food safety is discussed.

可可中的镉是哥伦比亚出口的主要障碍。因此，新兴技术需要提高可可的Cd检测能力。单色x射线荧光（MXRF）是一种具有成本效益的替代传统技术，如电感耦合等离子体（ICP-OES/MS）用于镉定量。MXRF可以应用于可可种植系统的固体或液体样品。虽然这种新技术已经证明了很高的准确性，但迄今为止还没有对主要分析参数进行验证。因此，本研究的目的是证明MXRF对可可和液体培养样品的适用性。采用土壤、土壤凋落物、根、茎、叶、豆荚、笔尖、壳和Luria-Bertani微生物培养基对方法进行验证。评估了Cd检测的稳健性、定量限（LOQ）、准确性、重复性、中间精密度和再现性。利用363个可可田间样品进行了MXRF和ICP之间的Cd相关性研究。统计分析表明，与ICP相比，MXRF的Pearson相关系数为0.96 ~ 0.99，回收率为74.8 ~ 129.9%。鲁棒性参数确定了适当的实验室和现场预处理。同样，60秒和200秒测量时间的选择也是至关重要的。定量限范围为0.124 ~ 0.148 mg kg−1。参数的正确率为90.7% ~ 109.0%。重现性的Z′-评分范围为- 0.50 ~ 0.62。验证了MXRF在可可体系和液体介质中Cd检测的适用性。讨论了这一新技术对可可和食品安全的影响。

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引用次数: 0