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RECENT DEVELOPMENTS IN ICPMS APPLIED TO STUDIES IN NUTRITION & HEALTH Steven F. Durrant 1 and Neil. I Ward 2 1 Laboratório de Plasmas Tecnológicos, Campus Experimental de Sorocaba, UNESP , Sorocaba, SP, Brazil 2 ICPMS Facility, University of Surrey, Guildford, Surrey, UK.
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APPLIED TO STUDIES
IN NUTRITION & HEALTH
Steven F. Durrant1 and Neil. I Ward2
1Laboratório de Plasmas Tecnológicos,
Campus Experimental de Sorocaba, UNESP,
Sorocaba, SP, Brazil
2 ICPMS Facility, University of Surrey, Guildford, Surrey, UK
Isotope ratio analysis
Wide linear dynamic range
Detection limits down to a few fgg-1
Low background count rates
Flexible magnetic sector instruments
Hazardous & time-consuming sample preparation
Limited precision for isotope ratio analysis (Quadrupole)
(Only) bulk analyses
Direct analysis of solids (conductors or insulators);
Little or no sample preparation;
High sample throughput;
Reduced water-related interferences;
Lower blank responses;
Reduced memory effects;
Spot, line, area or bulk analysis.
● Difficulty in obtaining fully quantitative analysis
● Poor precisions for isotope ratio measurements
(1) LA and SN to determine 235U:238U in the samples (S);(2) Nebulisation of isotopically-enriched tracer solution and simultaneous LA for the determination of 235U:238U in the mixture (X);(3) Nebulisation of isotope-enriched tracer (without LA) and measurement of the 235U:238U ratio in this solution (T). The elemental concentration was then obtained using
QS = QT(T – X)/[(X – S)mS/mT] where Q is concentration, and m is atomic mass.
● A concentration of 11.19 ± 1.11 μgg-1 was
determined in Apple Leaves
(Doped uranium concentration of 10 μgg-1).
● Low flow rate of the isotope-enriched tracer
● Easy and rapid analysis in any concentration range; the possibility to perform single-shot analysis.
Determination of Pb in whole blood
Application: Suspected pediatric lead poisoning
Traditional collection by finger of heel stick onto specially designed filter paper.
LA-ICP-TOF-MS with ablation using a CETAC LSX-213 system, λ = 213 nm, at 20 Hz, scan rate of 100 μms-1, φ = 200 μm.
Detection was with an Optimass 8000 ICP-TOF-MS (GBS Scientific Equipment Ltd, Australia).
(r2 = 0.996) but the analysis of Seronorm Whole Blood Reference Material yielded 5.6 ± 0.3 μgdl-1 compared to the 3.3 μgdl-1 reference value, i.e. the analysis was semi-quantitative.
● Reproducibility for individual blood spot scan data was typically about 7% RSD.
● A difficulty encountered was the different spreading characteristics of reconstituted freeze-dried CRMs compared to those of fresh blood.
International Journal of Mass Spectrometry 261 (2007) 199–207
Analytes 31P+, 32S+, 28Si+, 27Al+, 63Cu+, 64Zn+
Identification of phosphorylated subunits of yeast mitochondrial ATPase.
LA-ICPMS was then used to screen for P in the subunits. CETAC LSX 200, ELEMENT HR-ICPMS. S was used for internal standardization. P was determined in subunits Atp1p and Atp2p of the ATPase by MALDI-FTICR-MS
J. Sabine Becker, Miroslav Zoriy, J. Susanne Becker, Justina Dobrowolska and Andreas Matusch
J Anal Atom Spectrom, 2007, 22, 736-744
● Matrices: Teeth, hair, blood, nails, brain tissue, etc.
Single-cell analysis or analysis of organelles
● Theoretical depth resolutions of 5 nm are possible: 1mJ pulses at 266 nm.
● Barnes, JH, Schilling GD, Hieftje, GM, Sperline, RP, Bonner Denton, M, Barinaga, CJ, Koppenaal, DW, (2004) J Am Mass Spectrom, 15, 769-776.
Paquette, JL, Tiepolo, M (2007) Chem. Geol. 240:222-237.
Improved lateral resolution down to the hundred nm scale using the near-field effect induced by a silver needle positioned extremely close to the sample surface.
Becker, JS, Gorbunoff, A, Zoriy, M, Izmer, A, Kayser, M (2006) J Anal At Spectrom 21:19-25.
● SFD thanks the Brazilian agency FUNDUNESP for financial support