Detection of Al 2 O 3 particles in toothpaste by FFF- ICP-MS (confirmatory method)
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1 Detection of Al 2 O 3 particles in toothpaste by FFF- ICP-MS (confirmatory method) Manuel Correia, Katrin Loeschner National Food Institute, Technical University of Denmark (DTU) manco@food.dtu.dk NanoDefine Outreach Event Brussels, September 2017 NanoDefine is funded by the European Community's Seventh Framework Programme under Grant Agreement
2 Background Why Al 2 O 3 particles in toothpaste? Relevant in terms of risk assessment and labelling for cosmetics Al 2 O 3 particles not widely covered in other projects Complex mixture containing different types of nano/micro-particles (e.g. SiO 2, Al 2 O 3 ) Aims of the work: Develop a suitable sample preparation method for analyzing Al 2 O 3 in toothpaste by FFF-ICP-MS Develop the FFF-ICP-MS method and determine particle size and number concentration of Al 2 O 3 particles in toothpaste 2
3 Characteristics of the test toothpaste SiO 2 (abrasive) Al 2 O 3 (abrasive) TiO 2 (pigment) Ingredients: Aqua, Hydrated Silica, Sorbitol, Alumina, Olaflur, Hydroxyethylcellulose, Aroma, PEG-40 Hydrogenated Castor Oil, Stearic Acid, Sodium Saccharin, Cocamidopropyl Betaine, Citric Acid, Limonene, CI 77891, 3- (N-hexadecyl-N-2-hydroxiethylammonio)propyl-bis(2-hydroxiethyl)ammoniumdifluorid (1400 ppm F-) Al 2 O 3 TiO 2 SiO 2 Concentration (mg/g, N=3) Crystall. phases (XRD, BAM) Crystall. size (nm, XRD, BAM) ± ± ± 6.8 Corundum Anatase Courtesy of BAM
4 Pre-characterization of the toothpaste DLS and zeta-potential TEM-EDX Zave = 267 nm Zeta pot: -42 mv Complex and polydisperse NP mixture Proper separation and identification of the different NPs is required FFF-ICP-MS Toni Uusimäki, EAWAG 4
5 FFF-MALS/ICP-MS method development Sample preparation Tested on-line detectors Matrix dilution Chemical oxidation with H 2 O 2 AF4 separation parameters Carrier liquid (SDS, FL70, etc) Channel and membrane charact. Cross flow rate Focus/injection parameters Injected mass UV-vis absorption Dynamic light scattering (DLS) Multi angle light scattering (MALS) ICP-MS ICP-MS required for elementspecific information! 5
6 Results: Sample preparation Matrix dilution vs Chemical oxidation with H 2 O 2 (MALS data) Matrix dilution: unusual elution profile for and lower overall MALS signal Chemical oxidation: ~60% recovery in comparison to flow injections (based on light scattering) Chemical oxidation with selected as sample preparation procedure for analysis by FFF-MALS-ICP-MS 6
7 Results: AF4-MALS and AF4-ICP-MS Toothpaste after H 2 O 2 digestion, m inj = 10 µg MALS ICPMS ( 27 Al) Three particles types (SiO 2, Al 2 O 3 and TiO 2 ) contribute to the light scattering elemental specific detection by ICP-MS is required 7
8 Results: FFF method development Optimization of FFF conditions (for optimal recovery and conversion to number distributions (noise level, removal of void peak) Carrier liquid composition Cross-flow optimization Other parameters tested: membrane composition, carrier liquid (SDS, FL70, focus conditions), injection mass/volume 8
9 Results: FFF method performance Good reproducibility (6 different membranes) Linear response (5, 10, 25 µg inj. toothp.) Method can provide reproducible AF4-ICP-MS fractograms for Al 2 O 3 Drawback: low Al recoveries % AF4-ICPMS recovery (losses to membrane, large particles) 9
10 Results: FFF method performance Conversion to number-based particle size distribution Mass-based PSD Number-based PSD Artifact Presence of artifact in mass-based PSD (no particles detected by sp- If log-normal fit is applied d ICPMS after analysis of AF4 50 = 155 nm, analysed Al fractions log-normal 2 O 3 not consid. nanomaterial fit) 10
11 Summary and conclusions A FFF-ICP-MS method was sucessfully developed for separating and analyzing unknown Al 2 O 3 particles in toothpaste Mass recoveries were not satisfactory in certain cases this is difficult to avoid (loss of large particles) Secondary confirmatory method is required (e.g. artifacts) FFF-ICP-MS requires fine tuning for specific particle/matrix combinations 11
12 Thank you for your attention! Research Group for Nano-Bio Science New address since Easter 2017: DTU s new building for Life Science & Bioengineering This project has received funding from the European Union s Seventh Programme for research, technological development and demonstration under grant agreement No Toni Uusimäki 12
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