Title: Detection of titanium nanoparticles in human, animal and infant

Overview

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of Ti in milk. We analyzed infant formula (IF) and dairy livestock milk (Table S1). IF samples
thickened or not, organic-based or not (Table S2). Dairy livestock powder milk (PM) was raw or
(Table S1-2). Given that ICP-MS detects soluble Ti, we mineralized milk samples by double nitric-
which was much lower in PM (0.68 +/- 0.54 µg/L (Fig.1A)). Of note, Ti concentration was similar
and cow farm 2 “cow-F2”, table S1); organic raw milk from a donkey in Ariège county
located 200 km from Paris, FR (Table S1-2). XRF analysis at 5.1 keV with an unfocused beam
samples was however not observed for IF4 (Ti AUC=5.28 +/- 4.2, n=2 regions, Fig. S6A), a
analyzed human (n=8), IF (n=4) and livestock (n=3) milk samples (Fig. 2, S8-11). Our results
whose Ti hotspots were all rather dim. Hotspots sizes ranged from 1 pixel to 227, 118 and 531
equal or smaller than the beam size (3.1x2.6 µm). This 1-pixel sized population represented 5% of
total hotspots in farm cow milk up to 22% in human sample (Cow-F1-RW vs. H10, Fig. 2E,), and
in average 13 +/- 2.8% in human, 10+/- 1.3% in IF and 9 +/- 3.8 % in animal milk samples. Taken
13). Of the 119 hotspots analyzed, the great majority (94%) resulted in a Ti speciation.
13). Rutile TiO2 accounted for the majority of the Ti minerals detected (65% of total hotspots
analyzed) while anatase was the second most represented Ti bearing mineral (17% of total
hotspots). Ilmenite represented 5% of total hotspots and PB or titanite in 2%, while the mineral
bearing Ti remained not determined for 12% of hotspots analyzed (“nd”) (Fig. 3C). Sample-by-
any other milk sample analyzed. Anatase, which represented 17% of all the hotspots in human
bearing minerals was as follows: (%rutile:anatase:ilmenite:PB:nd): animal (73:10:0:2:15), human
larger clumps (IF1, IF1’, IF5, IF5’, and IF8, Table S3) or heated and sonicated for those that were
Ti-NPs represented a third of the total Ti particles detected (average 31.9 +/ 7.5 %, Fig. 4B). Some
In dairy livestock PM, Ti-NPs represented 38.3 +/- 7.8% of the total Ti particles (Fig. 4B and Table
A solution of 10 µg/L TiO2-NP standard reference material (Titanium Dioxide Nanomaterial 1898,
below 100 nm (Table S3) in accordance with the certificate of analysis for a non-sonicated solution
S16B, table S3), a concentration that was increased upon ultrafiltration to 4.6 x 106 part/L
TiO2-NPs 59. Sonication of the NIST standard induced a decrease of the Ti particle median size
and after sonication respectively that corresponds to a fold change of 4.8 (Table S3). Similar trends
were observed upon sonication of IF3 and IF5’ whose median particle size decreased from 146 to
IF3 and by 2.5-fold for IF5’ (Table S3). Finally, the contribution of soluble vs. particle Ti to the
total Ti concentration varied between samples (Fig. 4E and Table S3).
Ultrapure nitric acid (67-69% HNO3 PlasmaPURE® Plus ref 250-039-171, SCP Science,
Villebon-sur-Yvette). Ultrapure hydrofluoric acid (47-51% HF PlasmaPURE® Plus ref 250-036-
Samples of milk analyzed are listed in Tables S1-2. Human milk samples were collected by the
at the morning milking on 18/03/2021 from Jersey cows (n=5) (“Jersey”), Normande cows (n=6,
goat milk (Poland), raw cow milk (Austria) (Table S1). Infant formula (IF) milk was purchased
over the energy range of 4.95 to 5.05 keV with an equivalent energy step of 0.2 eV and an
solution of standard TiO2-NP (NIST) by single nanoparticle ICP-MS. (A) Ti particle size, (B) %
Donkey NIST 10µg/L

Methods (brief)

Gazeau5, Hervé Acloque4, Sophie Parat7, Joël Poupon3 and Anne Burtey4*.
nano-particles were detected in all samples, regardless of the species, location, and processing. We
digested milk samples by ICP-MS 47, hence without providing evidence for the presence of Ti as
(determination of chemical species), and size in the micro- and in nano-range, of Ti in samples of
First, we used Inductively Coupled Plasma Mass Spectrometry (ICP-MS) to evaluate the presence
of Ti in milk. We analyzed infant formula (IF) and dairy livestock milk (Table S1). IF samples
(Table S1-2). Given that ICP-MS detects soluble Ti, we mineralized milk samples by double nitric-
hydrofluoric acid digestion to release Ti from Ti-containing particles. As shown in Fig. 1A, Ti was
detected in all the IF samples tested and in 1 out of 5 PM samples. The concentration of Ti in IF
samples ranged from 1.13 to 50.72 µg per liter of milk, with an average of 13.35 +/- 3.85 µg Ti/L
Fig. 1A). To verify that the absence of detection of Ti in some samples was not due to a suboptimal
confirmed in all milk samples, even in those with low Ti concentration. An example is given in
milk samples. Milk samples that were not already in powder were freeze-dried and pressed into
pellets. In addition to the aforementioned milk samples, we analyzed breastmilk samples from ten
women living in Paris and its immediate suburbs (collected by the Lactarium Port-Royal, AP-HP,
Paris, FR). We also analyzed additional animal milk samples including raw (RW) or skimmed
revealed the bulk elemental composition of milk samples 52 (Fig. 1B and S2). The relative
(K), silicon (Si), calcium (Ca), phosphorus (P) varied between samples (Fig. 1B-C and S2-3), even

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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