Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder

Cocoa is a major commodity in the global food industry. Heavy metal contamination, particularly cadmium (Cd), raises significant concerns. This work demonstrates the use of laser-induced breakdown spectroscopy (LIBS) for fast Cd quantification in commercial cocoa powder across a wide range of concen...

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Main Authors: Juan Molina M., Raquel Pincay, Víctor Santos, José Luis González, María Fernanda Trujillo Guerrero, Diego Díaz Pace, César Costa-Vera
Format: Article
Language:English
Published: MDPI AG 2025-04-01
Series:Sensors
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Online Access:https://www.mdpi.com/1424-8220/25/8/2434
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author Juan Molina M.
Raquel Pincay
Víctor Santos
José Luis González
María Fernanda Trujillo Guerrero
Diego Díaz Pace
César Costa-Vera
author_facet Juan Molina M.
Raquel Pincay
Víctor Santos
José Luis González
María Fernanda Trujillo Guerrero
Diego Díaz Pace
César Costa-Vera
author_sort Juan Molina M.
collection DOAJ
description Cocoa is a major commodity in the global food industry. Heavy metal contamination, particularly cadmium (Cd), raises significant concerns. This work demonstrates the use of laser-induced breakdown spectroscopy (LIBS) for fast Cd quantification in commercial cocoa powder across a wide range of concentrations (70–5000 ppm). Cocoa powder presents unique challenges due to its physical properties, such as the tendency to soften and liquefy at elevated temperatures, which complicates sample preparation. To address these issues, a mechanical mixing and pelletization protocol was implemented to ensure uniformity. Pellets were doped with known cadmium concentrations for calibration. Cadmium atomic lines at 340.36 and 361.05 nm were used to construct quantification curves. A special algorithm for background subtraction was implemented, and the LIBS plasma was characterized to ensure local thermodynamic equilibrium conditions. Out of eighteen samples, five double-blinded unknowns were evaluated. The concentrations agreed well within normalized standard deviations of 9.73% and 5.88% for the two cadmium lines. The limits of detection for the lines were 0.4 and 0.08 μg/g, respectively. LIBS is confirmed as a rapid and versatile analytical tool for Cd detection and quantification in complex food matrices, with potential applications in field-based and industrial monitoring systems.
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spelling doaj-art-ea9f8ca9b1464b12aa9fcb950d1740a22025-08-20T03:13:53ZengMDPI AGSensors1424-82202025-04-01258243410.3390/s25082434Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa PowderJuan Molina M.0Raquel Pincay1Víctor Santos2José Luis González3María Fernanda Trujillo Guerrero4Diego Díaz Pace5César Costa-Vera6Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Calle Godoy Cruz 2290, Buenos Aires 1425, ArgentinaMass Spectrometry & Optical Spectroscopy Group, Departamento de Física, Escuela Politécnica Nacional (EPN), Ladrón de Guevara E11–253, Ed. #6, Piso 1, Quito 170525, EcuadorDepartamento de Automatización y Control Industrial, Escuela Politécnica Nacional, Ladrón de Guevara E11-253, Quito 170525, EcuadorMass Spectrometry & Optical Spectroscopy Group, Departamento de Física, Escuela Politécnica Nacional (EPN), Ladrón de Guevara E11–253, Ed. #6, Piso 1, Quito 170525, EcuadorDepartamento de Automatización y Control Industrial, Escuela Politécnica Nacional, Ladrón de Guevara E11-253, Quito 170525, EcuadorConsejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Calle Godoy Cruz 2290, Buenos Aires 1425, ArgentinaMass Spectrometry & Optical Spectroscopy Group, Departamento de Física, Escuela Politécnica Nacional (EPN), Ladrón de Guevara E11–253, Ed. #6, Piso 1, Quito 170525, EcuadorCocoa is a major commodity in the global food industry. Heavy metal contamination, particularly cadmium (Cd), raises significant concerns. This work demonstrates the use of laser-induced breakdown spectroscopy (LIBS) for fast Cd quantification in commercial cocoa powder across a wide range of concentrations (70–5000 ppm). Cocoa powder presents unique challenges due to its physical properties, such as the tendency to soften and liquefy at elevated temperatures, which complicates sample preparation. To address these issues, a mechanical mixing and pelletization protocol was implemented to ensure uniformity. Pellets were doped with known cadmium concentrations for calibration. Cadmium atomic lines at 340.36 and 361.05 nm were used to construct quantification curves. A special algorithm for background subtraction was implemented, and the LIBS plasma was characterized to ensure local thermodynamic equilibrium conditions. Out of eighteen samples, five double-blinded unknowns were evaluated. The concentrations agreed well within normalized standard deviations of 9.73% and 5.88% for the two cadmium lines. The limits of detection for the lines were 0.4 and 0.08 μg/g, respectively. LIBS is confirmed as a rapid and versatile analytical tool for Cd detection and quantification in complex food matrices, with potential applications in field-based and industrial monitoring systems.https://www.mdpi.com/1424-8220/25/8/2434laser-induced breakdown spectroscopyLIBScadmiumcocoa
spellingShingle Juan Molina M.
Raquel Pincay
Víctor Santos
José Luis González
María Fernanda Trujillo Guerrero
Diego Díaz Pace
César Costa-Vera
Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
Sensors
laser-induced breakdown spectroscopy
LIBS
cadmium
cocoa
title Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
title_full Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
title_fullStr Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
title_full_unstemmed Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
title_short Assessing the Sensitivity and Efficiency of Laser-Induced Breakdown Spectroscopy (LIBS) for High-Concentration Cadmium Detection in Cocoa Powder
title_sort assessing the sensitivity and efficiency of laser induced breakdown spectroscopy libs for high concentration cadmium detection in cocoa powder
topic laser-induced breakdown spectroscopy
LIBS
cadmium
cocoa
url https://www.mdpi.com/1424-8220/25/8/2434
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