approach to speciation analysis. As in previous years, As speciation continues to dominate the

Overview

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Key numbers

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4.4 Metallodrug Speciation… 81
row transition elements, notable Ni and V28. The reviewers identify the key advances to be the
metal-containing species ion, a resolving power above one million and a mass accuracy of 0.05 ppm
fraction of MeHg is 0.125 µg kg-1 (as Hg) which is 0.16% of the total Hg content. The mass fractions
Behnken design, the optimal response was achieved using 0.5% NaBH4, 1.5 mol L-1 HCl and a 40 µL
elution volume. A retention efficiency of > 99% was achieved with a preconcentration factor of 100.
The LOD and LOQ were 0.4 and 1.2 ng L-1 respectively with an RSD of 7.9% (n = 10) with an analysis
reference levels, measured by HPLC-AFS, were detected in drinking water (70% of n = 83 total
samples), foods (80%, n = 188), urine (95%, n = 63), saliva (44%, n = 48), hair (80%, n = 51) and nails
metals. Methylated Sb species were predominant in urine (46-100%) and saliva (74-100%) in
over 93% of Sb in rat blood was integrated into Hb. The Sb retained in liver homogenate
samples were SbV, Sb2O5, and metallic Sb, SbIII was not observed. Table 1 shows other applications
alkylated AsV compounds was quantified using ICP-OES with an expanded uncertainty ≤ 2.4 %. These
and within 12 min on a 25 cm strong anion exchange column. The LOD values obtained were 0.9-
of 87-102%. A sp-ICP-MS method has been utilised for analysis of the physical forms of As in
recording or multiple reaction detection. The LOQ values for the techniques described were 454 µg
kits. The RSD was 7.1% (n = 8). The method was validated against the CRM ERM (R)-CA615
efficiencies in the range 13-30% most probably due to a complicated mechanism of HG. While the
factor of 972 was achieved with a LOD of 0.045 ng mL-1. The incorporation of active nanomaterials
the automated system offered LOD values of 0.004-0.033 µg L-1 for As and 0.061-0.128 µg L-1 for Se.
methanol contents, indicating a compound dependent response. Further tests with a 25% methanol
almost 80%. The total As concentration throughout the profile ranged between 0.2 and 9.8 mg kg -
1. Organic As species (DMA + MMA + TMAO + AB) accounted, on average, for 28 ± 10% of the total
As (range: 6-51%), and for 37 ± 13% of the extracted As (range: 7-64%). The relative abundance of
samples of the inner region (mean = 1.5 µg As L-1) were significantly lower than in those of the outer
region (mean = 5.2 µg As L-1). Conversely, concentrations of As in suspended particles in the inner
region (mean = 14 µg As g-1) were much greater than in the outer region (mean = 5.7 µg As g-1). The
range 0.04 - 0.07 ng mL-1. Three unknown As species were also recorded, one of which was a kind
proportions of inorganic As (>99%) were found in two As-hyperaccumulating ferns, Pteris vittata
proportions of 51- 53% AsIII and 38-48% AsV. The only organic species present in the earthworm
samples was AB, although at low proportions (<9%). The internal bioconversion of other As species
WDXRF, ranged from 145 to 40,200 mg kg-1. Analysis by XRD showed the presence of jarosite and
ash) in four particle size ranges from PM<1 – PM>10 have been used to study the distribution and
was 90-98% of the total As. The As concentrations and speciation in wild birds on an abandoned As
species as the dominant (>92%) As species. Further analysis of the bird samples using XANES
efficiencies (96-104%) and recoveries of As species in rice (95-100%) were good. Interconversion
nanoparticles significantly reduced the accumulation of AsIII in rice roots by 88 and 97% and in rice
shoots by 71 and 77% when the initial As was supplied as AsIII and AsV, respectively. The ZnO
nanoparticles also reduced AsV in rice roots by 68 and 52% when the As was provided as As III and
1.1, and 0.1 with mobile phases A and B also containing 1% methanol), four As species (As III, AsV,
Switzerland has been studied by Guillod-Magnin et al.69. An IC-ICP-MS method was developed to
products, except for rice drinks, was AsIII, comprising 60-80% of the total As content, followed by

Methods (brief)

4.4 Metallodrug Speciation… 81
and geological metallomics (188 references). Sample preparation and some strategies for
description of methods based on HPLC coupled with both/either ICP-MS and ES-MS. A shorter
analytical methods incorporating MS, such as elemental ICP-MS and molecular Q-TOF-MS, generally
coupled with multidimensional chromatography, and LA-ICP-MS. Several examples of applications
instrumental techniques including single-cell ICP-MS, mass cytometry, LA-ICP-MS, synchrotron XRF
Several reviews feature the central role of ICP-MS, particularly when combined with LC separations.
for a range of chromatographic separation techniques with on-line elemental detection by ICP-MS
tagged with exogenous metals18. The reviewers discuss the challenges of sample preparation for
designs and improved detectors. It is predicted that ICP-QQQ-MS will emerge as a viable alternative
for the determination of difficult analytes that previously required expensive HR-ICP-MS and that
part of the review deals with the determination of APIs that contain an ICP-MS-quantifiable
quantifiable by ICP-MS. This section is further subdivided by functional group (hydroxyl, carboxyl,
thiol, and amino). The reviewers note that the application of HPLC-ICP-MS is still far from routine in
tandem ICP-MS/MS has revolutionised the determination of the most important hetero-elements
The determination of F is also discussed by Feldmann et al.20 in a tutorial review (49 references) of
increasingly met by simpler and cheaper procedures that do not involve ICP-MS, or even HPLC. By
sample. The problems of compound-dependent responses are discussed and the value of ICP-MS in

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