Lo Dico et al. 2015 - ICP-MS metals in infant formula

Lo Dico and colleagues validated an ICP-MS method for simultaneous determination of arsenic, copper, chromium, selenium, tin, cadmium, antimony, and lead in infant formula after microwave-assisted digestion. The paper is a pure method-validation study and does not report measured concentrations of the eight elements in the 10 commercial liquid-milk infant formulas collected from Sicilian supermarkets in February–March 2015. Those 10 samples served as the matrix for spike-recovery experiments. The paper reports total elements only and does not perform arsenic, chromium, tin, or mercury speciation. The source contributes ICP-MS method-validation context to infant-formula testing-method discussions; it does not contribute occurrence values to the standards pool.

Key numbers

• Target analytes: As, Cu, Cr, Se, Sn, Cd, Sb, and Pb.
• Sample collection: 10 commercial liquid-milk infant formulas from four popular brands, collected across Sicily between February and March 2015, targeted for infants aged 6 to 12 months. No measured concentrations in these samples are reported in the paper.
• Multielement calibration solutions were prepared at concentrations from 0.001 to 50 µg/L; the working calibration curve used 8 standard additions (BlankCal, 0.01, 0.05, 0.1, 0.5, 1, 5, 10, 50 µg/L) with r² ≥ 0.999 (paper page 2–3).
• Method LoDs and LoQs (Table 6, mg/kg): As LoD 0.001 / LoQ 0.002; Cd LoD 0.0008 / LoQ 0.001; Pb LoD 0.002 / LoQ 0.006; Sb LoD 0.003 / LoQ 0.008; Se, Cr, Sn, Cu LoD 0.50 / LoQ 1.00. Applicability range upper bound 2.50 mg/kg for all eight elements.
• CRM validation (Table 2, Fapas T07183QC infant cereal): Cd certified 0.047 ± 0.005 mg/kg vs measured 0.048 ± 0.003 mg/kg; Cr 0.135 ± 0.020 vs 0.132 ± 0.010; Pb 0.066 ± 0.010 vs 0.067 ± 0.004; Se 0.085 ± 0.010 vs 0.084 ± 0.009.
• Recovery across all elements at three spiked levels: 96–105 %.

Methods (brief)

ICP-MS on an Agilent 7700x series instrument with an ASX-500 autosampler and a water-cooled quartz cyclonic spray chamber. Sample digestion used an Anton-Paar Multiwave 3000 microwave digester with eight MF100 PTFE-TFM vessels, per UNI EN 13805:2002: 1 g sample plus 3 mL of 60 % ultrapure nitric acid (Merck KGaA) and 5 mL of water. Accuracy was verified against Fapas test material T07183QC (infant cereal). Validation parameters covered selectivity, recovery, repeatability, within-laboratory reproducibility, instrumental and method LoDs/LoQs, range of linearity, and standard measurement uncertainty per Commission Regulations EC 333/2007, EC 836/2011, EC 488/2014, and EC 1881/2006.

Implications

Certification: Method-validation context only. This source does not contribute occurrence values to the standards pool because no measured market-sample concentrations are reported; routing should reflect testing-method context rather than direct evidence on infant-formula product pages.

Courses: Useful as a documented example of a microwave-digestion plus ICP-MS workflow for infant formula, with explicit alignment to EC 333/2007 and EC 836/2011 official-control criteria.

App: No occurrence data to surface; the source informs methodology references rather than consumer-facing concentration estimates.

Wiki pages this source may touch

• Infant Formula
• Infant Formula
• Arsenic, Total
• Cadmium
• Lead
• Chromium
• Tin
• Antimony

Verification notes

The same DOI was fetched under formula and infant-formula Cd, Pb, Sn, and tAs gaps. This page is the canonical page for those duplicate paths. Arsenic, chromium, tin, and mercury are total-element measurements; no iAs, Cr(VI), inorganic-Sn, or MeHg speciation is performed. Cu and Se are reported in the source but are outside the HMTc analyte vocabulary and are not surfaced in the metals: frontmatter. The paper measured liquid-milk (RTF) infant formula only; powder, concentrated-liquid, and soy-based subcategories are not in scope.

Page history

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