instrumentation for monitoring toxic elements in food matrices:

Overview

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Key numbers

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for ICP-MS analysis. Estimated LODs in μg/g (ppm) were: Pb, 0.06; Tl, 0.06; Hg, 0.06; Cd, 0.04; and Sn, 0.11.
background noise (Chen et al., 2008; Chen and Wittry, 1998). Portable The principal goals of this study were: (1) to evaluate the perfor
optimizing the Bragg condition at a wider range of incident angles. the Niton™ XL3t GOLDD and Niton™ XL5 Plus analyzers (ThermoFisher
modate a low-power X-ray source as well as a means for quickly The Zmax™ uses an X-ray tube operated at 35W and a single DCC optic
practices (Acheampong et al., 2024; Akhbarizadeh et al., 2023). Despite optimal Limits of Detection (LOD)s for the elements Pb, Hg, As, Se, and
analysis (Pb, Cd, and Tl); chicken cordon bleu samples (n = 8) circulated
Sn); and catfish fillet samples (n = 8) circulated in FY2024 (2024-FERN)
from Colombia: Cardamom (Elettaria cardamomum) (n = 1), Chamomile film, using light pressure to create a thin sample. The entire sample cup
(Matricaria chamomilla) (n = 1), Eucalyptus (Eucalyptus spp.) (n = 1), and the second film were secured by a plastic ring (Fig. 2a). The Zmax™
Hibiscus Flower (Hibiscus sabdariffa) (n = 1), Holy Basil (Ocimum ten sample cup is designed to achieve an ~0.2-mm sample thickness sand
(Calendula officinalis) (n = 1); 2) Thirty dried spice samples from the sample.
Colombian and the US markets: Parsley (Petroselinum crispum) (n = 2), In contrast, the sample cup arrangement for analysis on the Emax™
Achiote (fruit, Bixa orellana) (n = 1), Allspice (fruit, Pimenta dioica) (n = utilizes plastic cup with a flat Prolene® X-Ray thin film window at one
1), Dreaming seasoning (spice blends) (n = 1), Black pepper (fruit, Piper end. Approximately 0.5 – 1g of sample is transferred into the Emax™
nigrum) (n = 1), Chili Sakthi (Spice blends) (n = 1), Cinnamon (bark, cup, which is secured with a plastic clip. For the Emax™ the energy of
Coriander (Coriandrum sativum) (n = 3), Curry (Murraya koenigii) (n = be used to obtain a higher Cd fluorescence intensity. (Fig. 2b).
1), Flavor Forward (Spice blends) (n = 1), Garam-Masala (Spice blends)
L.) (n = 1), Mural of flavor (herby blends) (n = 1), Nutmeg (Myristica
fragrans) (n = 1), Oregano (Origanum vulgare) (n = 4), Potato weed 3.1. Limits of detection for XRF analyzers
(Galinsoga parviflora) (n = 2), Red chili pepper (Capsicum annuum) (n =
1), Rosemary (Rosmarinus officinalis) (n = 1), Thyme (leaf, Thymus vul The LODs for the Zmax™ and Emax™, the HD Mobile® and the two
garis) (n = 2), and Turmeric (Curcuma longa) (n = 1). Niton™ XRF analyzers are provided in Table 1. The LOD data for the
CRMs were analyzed directly on the Z-Spec XRF instruments (s) at low levels in a relevant food matrix (n ≥ 6). The LOD is calculated
Emax Zmax HD Mobile Niton XL3t Niton 5+ mented (i.e., spiked); with 150 μg/kg of Pb, Cd, and Tl; and (c) three
samples supplemented with 1000 μg/kg of Pb and Tl (Table 3). As ex
Ca 240 15 LOD for Pb, Cd, and Tl in the “un-spiked” control samples. For the
Cd 0.04 11 6 5 samples “nominally” spiked with 150 μg/kg, XRF recoveries ranged
from 98.1 % to 109 % for the three metals, while precision (defined as
Hg 0.15 0.06 1 2 1 the samples “nominally” spiked with 1000 μg/kg Pb and Tl, recoveries
W 0.2 0.1 spiked with 150 μg/kg Pb, Tl, Hg, Cd, and 1000 μg/kg Sn; (c) three
Zn 10 0.1 2 5 samples spiked with 1000 μg/kg Pb, Tl, Hg, Cd, and 2500 μg/kg Sn
(Table 4). Due to the high levels of Sn supplemented into the FY23
supplementary material (Table S1). The default analysis routines for the
positive detection in the control samples for 26300 μg/kg for Sn. For the
samples nominally spiked at 150 μg/kg, recoveries ranged from 90.7 %
to 128 % for the Z-spec analyzers, while the repeatability ranged from
4.02 % to 13.5 %. For the Niton™ analyzers, all samples were non-
for the Z-Spec analyzers, and repeatability (CV) ranged from 1.16 % to
12.1 %; for Sn, which was spiked at 2500 μg/kg, recovery was 97 % with
1.82 % %CV. For the Niton™ analyzers all elements except Sn were non-
detects with the Sn recovery of 141.78 % and 65.31 % with 1.487 and
difference relative to the CRM assigned value they are within ±10 %,

Methods (brief)

optics has been used successfully for X-ray fluorescence (XRF) analysis of many different sample matrices.
consumer products, food, and cultural medications, with limits of detection (LOD) on the order of a single digit
for Cd in CRMs. Archived food-based proficiency test (PT) samples were analyzed to assess the performance of
the Zmax™ and Emax™ as screening tools to detect key elements. Some of the PT samples were also analyzed
using the two Niton™ XRF instruments as well as the HD Mobile® for comparison purposes. These PT samples
from analyses based on Inductively Coupled Plasma Mass Spectrometry (ICP-MS). For the FERN 2022 PT samples
for ICP-MS analysis. Estimated LODs in μg/g (ppm) were: Pb, 0.06; Tl, 0.06; Hg, 0.06; Cd, 0.04; and Sn, 0.11.
Several ‘real-world’ samples were analyzed using the Zmax™ and Emax™ devices, including medicinal herbs
mining the elemental composition of a sample by measuring the in to even low levels of toxic metals such as Cd, Pb, Hg, and the metalloid
tensity of X-rays emitted when the sample is subjected to a suitable As, can result in bioaccumulation within the body and have been asso
EDXRF detects multiple elements simultaneously, with resolution such as atomic absorption spectrometry (AAS) and inductively coupled
contingent on detector performance. While WDXRF excels in plasma mass spectrometry (ICP-MS) are widely used for detecting and
element detection by minimizing interferences from other elements and and requires less skill to operate compared to AAS and ICP-MS.
toring requires rapid detection of toxic elements in diverse samples, (Fig. 1) are equipped with DCC optic(s) for M-XRF excitation (Chen
M-XRF for field-based studies was the HD-Mobile® (X-ray Optical Sys terest in the sample. A fast silicon-drift detector (SDD) captures the
purpose. Beyond their use as food flavorings, some spices also play a count rate for each the elements detected in the sample. Then these net
practices (Acheampong et al., 2024; Akhbarizadeh et al., 2023). Despite optimal Limits of Detection (LOD)s for the elements Pb, Hg, As, Se, and
Tl. In contrast, the Emax™ is designed to achieve optimal LODs for Mo, run time. The detector was housed in a new Thermo Portable Test

Implications

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Update history

The five most recent substantive edits to this page, classified major (evidence or structure moved), correction (a published value or statement was wrong and has been fixed), or minor (narrative rewritten without changing the underlying evidence). Each description is derived from what the edit did to this page; the linked commit is the authoritative record, routine regeneration passes are excluded, and the full version history lives in git. When DOI minting comes online (see schema docs), each entry below will also link to a version-pinned DataCite DOI.

Commit	Date	Change	Description
b01ec52c	2026-08-04	major	2 sections added
d49e450f	2026-08-03	major	5 sections added; narrative text revised