Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee

A rapid and efficient ultrasound-assisted extraction (UAE) procedure followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of 14 rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu), along with yttrium (Y) and scandium (S...

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Main Authors: Aleksandra Savić, Jelena Mutić, Milica Lučić, Jelena Vesković, Andrijana Miletić, Antonije Onjia
Format: Article
Language:English
Published: MDPI AG 2025-01-01
Series:Foods
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Online Access:https://www.mdpi.com/2304-8158/14/2/275
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author Aleksandra Savić
Jelena Mutić
Milica Lučić
Jelena Vesković
Andrijana Miletić
Antonije Onjia
author_facet Aleksandra Savić
Jelena Mutić
Milica Lučić
Jelena Vesković
Andrijana Miletić
Antonije Onjia
author_sort Aleksandra Savić
collection DOAJ
description A rapid and efficient ultrasound-assisted extraction (UAE) procedure followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of 14 rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu), along with yttrium (Y) and scandium (Sc), in coffee samples. The method was validated using certified reference material (NIST SRM 1547), recovery tests at four fortification levels, and comparisons with microwave-assisted digestion (MAD). Excellent accuracy and precision were achieved, with recovery rates ranging from 80.1% to 112% and relative standard deviations (RSD%) below 14%. Limits of detection (LODs) ranged from 0.2 ng/kg (Yb) to 0.16 µg/kg (Nd). Total REE concentrations varied between 8.3 µg/kg and 1.1 mg/kg, with the highest individual mean concentrations (µg/kg) observed for Ce (11.7), La (6.0), and Sc (4.7). The lowest individual mean concentrations (µg/kg) were for Ho (0.16), Lu (0.066), and Tm (0.063). Multivariate analysis of REE profiles from 92 coffee samples collected in Serbia revealed clear distinctions between ground roasted and instant coffees, as well as between different surrogate blends. This study indicated that the determination of coffee’s geographical origin was not possible due to the diverse types, blends, and additives. However, differences in REE profiles suggest potential classification based on variety. REEs pose a negligible health risk to coffee consumers, with HI values ranging from 4.7 × 10<sup>−8</sup> to 6.3 × 10<sup>−6</sup> and TCR ranging from 2.6 × 10<sup>−14</sup> to 3.5 × 10<sup>−12</sup>.
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institution Kabale University
issn 2304-8158
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spelling doaj-art-091d3940171647c8aabc6b406dfcbe022025-01-24T13:33:06ZengMDPI AGFoods2304-81582025-01-0114227510.3390/foods14020275Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in CoffeeAleksandra Savić0Jelena Mutić1Milica Lučić2Jelena Vesković3Andrijana Miletić4Antonije Onjia5Anahem Laboratory, Mocartova 10, 11160 Belgrade, SerbiaDepartment of Analytical Chemistry, Faculty of Chemistry, University of Belgrade, 11158 Belgrade, SerbiaInnovation Center of the Faculty of Technology and Metallurgy, 11120 Belgrade, SerbiaFaculty of Technology and Metallurgy, University of Belgrade, 11120 Belgrade, SerbiaFaculty of Technology and Metallurgy, University of Belgrade, 11120 Belgrade, SerbiaFaculty of Technology and Metallurgy, University of Belgrade, 11120 Belgrade, SerbiaA rapid and efficient ultrasound-assisted extraction (UAE) procedure followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of 14 rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu), along with yttrium (Y) and scandium (Sc), in coffee samples. The method was validated using certified reference material (NIST SRM 1547), recovery tests at four fortification levels, and comparisons with microwave-assisted digestion (MAD). Excellent accuracy and precision were achieved, with recovery rates ranging from 80.1% to 112% and relative standard deviations (RSD%) below 14%. Limits of detection (LODs) ranged from 0.2 ng/kg (Yb) to 0.16 µg/kg (Nd). Total REE concentrations varied between 8.3 µg/kg and 1.1 mg/kg, with the highest individual mean concentrations (µg/kg) observed for Ce (11.7), La (6.0), and Sc (4.7). The lowest individual mean concentrations (µg/kg) were for Ho (0.16), Lu (0.066), and Tm (0.063). Multivariate analysis of REE profiles from 92 coffee samples collected in Serbia revealed clear distinctions between ground roasted and instant coffees, as well as between different surrogate blends. This study indicated that the determination of coffee’s geographical origin was not possible due to the diverse types, blends, and additives. However, differences in REE profiles suggest potential classification based on variety. REEs pose a negligible health risk to coffee consumers, with HI values ranging from 4.7 × 10<sup>−8</sup> to 6.3 × 10<sup>−6</sup> and TCR ranging from 2.6 × 10<sup>−14</sup> to 3.5 × 10<sup>−12</sup>.https://www.mdpi.com/2304-8158/14/2/275ArabicaCanephorasurrogateREEsinductively coupled plasma mass spectrometrypositive matrix factorization
spellingShingle Aleksandra Savić
Jelena Mutić
Milica Lučić
Jelena Vesković
Andrijana Miletić
Antonije Onjia
Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
Foods
Arabica
Canephora
surrogate
REEs
inductively coupled plasma mass spectrometry
positive matrix factorization
title Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
title_full Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
title_fullStr Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
title_full_unstemmed Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
title_short Ultrasound-Assisted Extraction Followed by Inductively Coupled Plasma Mass Spectrometry and Multivariate Profiling of Rare Earth Elements in Coffee
title_sort ultrasound assisted extraction followed by inductively coupled plasma mass spectrometry and multivariate profiling of rare earth elements in coffee
topic Arabica
Canephora
surrogate
REEs
inductively coupled plasma mass spectrometry
positive matrix factorization
url https://www.mdpi.com/2304-8158/14/2/275
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