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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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RECENT DEVELOPMENTS IN ICPMS

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

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Inductively coupled plasma mass spectrometry (ICPMS)

Advantages

Multielemental analysis

Isotope ratio analysis

Solution-based calibration

High throughput

Wide linear dynamic range

Detection limits down to a few fgg-1

Low background count rates

Flexible magnetic sector instruments

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ICPMS

Disadvantages

Interferences

Matrix effects

Hazardous & time-consuming sample preparation

Limited precision for isotope ratio analysis (Quadrupole)

(Only) bulk analyses

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Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS)

Advantages

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.

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Laser ablation inductively coupled plasma mass spectrometry

Disadvantages

● Difficulty in obtaining fully quantitative analysis

● Poor precisions for isotope ratio measurements

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● Pickhardt, C, Izmer, AV, Zoriy, MV, Schumlöffel, D, Becker, JS (2006) Int J Mass Spectrom 248:136-141. ● Online isotope dilution was employed with LA-ICPMS. ● A microflow total consumption nebuliser DS-5 (CETAC Technologies, Omaha, NE, USA) was mounted in the ablation chamber.
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● A nebuliser solution uptake rate of 7 μlmin-1 was provided by a high precision syringe pump. ● To determine a doped uranium concentration in NIST SRM 1515 Apple leaves using a CETAC LSX 200 systemλ = 266 nm, 10 Hz, φ = 300 μm. ●A quadrupole ICPMS fitted with a collision cell was used for detection.
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Procedure

(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.

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An internal standardization procedure was employed to compensate for differences in sensitivity between LA- and SN-ICPMS.

Results

● A concentration of 11.19 ± 1.11 μgg-1 was

determined in Apple Leaves

(Doped uranium concentration of 10 μgg-1).

Advantages

● Low flow rate of the isotope-enriched tracer

● Easy and rapid analysis in any concentration range; the possibility to perform single-shot analysis.

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Cizdziel, JV (2007) Anal Bioanal Chem 388:603-611.

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).

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●Results: A linear calibration curve was obtained

(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.

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H. Sela, Z. Karpas, M. Zoriy, C. Pickhardt, J.S. Becker (2007) Biomonitoring of hair samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

International Journal of Mass Spectrometry 261 (2007) 199–207

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Krause-Bucholz, U, Becker, JS, Zoriy, M, Pickhardt, C, Przybylski, M, Rödel, G, Becker, JS (2006) Int J Mass Spectrom 248:56-60.

Analytes 31P+, 32S+, 28Si+, 27Al+, 63Cu+, 64Zn+

Identification of phosphorylated subunits of yeast mitochondrial ATPase.

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The complexes were separated in their native state in the 1st dimension (BN-PAGE) and their subunit composition resolved by SDS-PAGE in the 2nd dimension under denaturing conditions.

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

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Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in elemental imaging of biological tissues and in proteomics

J. Sabine Becker, Miroslav Zoriy, J. Susanne Becker, Justina Dobrowolska and Andreas Matusch

J Anal Atom Spectrom, 2007, 22, 736-744

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Applications

● Matrices: Teeth, hair, blood, nails, brain tissue, etc.

Elemental mapping

Proteomics

Single-cell analysis or analysis of organelles

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Performance (Resolution)

● 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.

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Lateral resolutions of 5 μm (zircon using a MicroLas GeoLas 102 ArF excimer laser, λ = 193 nm.

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.

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Acknowledgements

● SFD thanks the Brazilian agency FUNDUNESP for financial support

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