scholarly journals Simultaneous Determination of Chromium, Selenium, and Molybdenum in Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: Single-Laboratory Validation

2011 ◽  
Vol 94 (4) ◽  
pp. 1240-1252 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Andre Szabo ◽  
Joseph T Thompson

Abstract An inductively coupled plasma/MS method was developed for the simultaneous determination of Cr, Se, and Mo in infant formulas and other nutritional products. All samples were digested using a closed vessel microwave oven system, together with Ni and Te internal standards. The practical quantitation limits for Cr, Se, and Mo were 0.4, 0.2, and 0.4 ng/mL, respectively; dilution factors were 250 for powders and 50 for liquids. The Cr, Se, and Mo concentrations in 10 nutritional products were within specifcation limits, and within-day and day-to-day (6 independent days) precision values were <5% RSD. For two control samples, the observed precision was ≤2% RSD over 10 independent days. In three National Institute of Standards and Technology standard reference materials, Cr, Se, and Mo results were within the certifed limits. The average sample spike recoveries for 10 nutritional products ranged from 93 to 107%. Robustness studies showed a minimal effect from concomitant easily ionized element concentrations. However, the choice of internal standard and matrix matching carbon content were critical to obtaining accurate Se results. All indications are that this method would be a suitable candidate as a global reference method for the determination of these trace elements in nutritional products.

2012 ◽  
Vol 95 (3) ◽  
pp. 588-598 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Andre Szabo ◽  
Joseph J Thompson ◽  
Steve Baugh

Abstract An inductively coupled plasma/MS method was developed for the simultaneous determination of Cr, Se, and Mo in infant formula and other nutritional products. All samples were digested using a closed vessel microwave oven system, together with Ni and Te internal standards. The practical quantitation limits for Cr, Se, and Mo were 0.4, 0.2, and 0.4 ng/mL, respectively; dilution factors were 250 for powders and 50 for liquids. The Cr, Se, and Mo concentrations in 10 nutritional products were within specification limits; within-day and day-to-day (6 independent days) precision values were <5% RSD. For two control samples, the observed precision was ≤2% RSD over 10 independent days. Cr, Se, and Mo results were within the certified limits in three National Institute of Standards and Technology standard reference materials. The average sample spike recoveries for 10 nutritional products ranged from 93 to 107%. Robustness studies showed a minimal effect from concomitant easily ionized element concentrations. However, the choice of internal standard and matrix-matching carbon content were critical to obtaining accurate Se results. All indications are that this method would be a suitable candidate as a global reference method for the determination of these trace elements in infant formula, adult nutritionals, and other nutritional products.


2004 ◽  
Vol 50 (7) ◽  
pp. 1214-1221 ◽  
Author(s):  
Sichun Zhang ◽  
Chao Zhang ◽  
Zhi Xing ◽  
Xinrong Zhang

Abstract Background: An inductively coupled plasma mass spectrometry (ICP-MS)-based immunoassay has been proposed independently by Baranov et al. (Anal Chem 2002;74:1629–36) and our group, but the applicability of this method for multianalyte analysis in clinical samples has not been fully illustrated. We developed a dual-label immunoassay method for the simultaneous determination of α-fetoprotein (AFP) and free β-human chorionic gonadotropin (hCGβ) in human serum. Methods: Monoclonal antibodies immobilized on microtiter plates captured AFP and hCGβ, which were detected by use of Eu3+-labeled anti-AFP and Sm3+-labeled anti-hCGβ monoclonal antibodies. Eu3+ and Sm3+ were dissociated from the immunocomplex with HNO3 solution (10 mL/L) and delivered by peristaltic pump to the ICP mass spectrometer. Results: The measurable ranges of AFP and hCGβ were 4.6–500 and 5.0–170 μg/L, respectively, with detection limits of 1.2 and 1.7 μg/L (3 SD above mean of zero calibrator), respectively. The intraassay imprecision (CV) for AFP was 8.3%, 4.0%, and 2.7% at 16.3, 86, and 354 μg/L, respectively, and the interassay CV was 10%, 5.7%, and 3.5%. For hCGβ, the intraassay CV was 5.4%, 6.4%, and 3.1%, respectively, at 10.5, 45.2, and 105 μg/L, and the interassay CV was 7.2%, 8.0%, and 3.7%. Comparison with IRMAs for AFP and hCGβ yielded correlation coefficients (r2) of 0.97 and 0.95. Conclusions: Two proteins can be measured simultaneously by immunoassays using two rare earth elemental tags (Eu3+ and Sm3+) and ICP-MS detection. The multielement capability and the multiple potential elemental labels make ICP-MS attractive for multianalyte immunoassays. Implementation of ICP-MS-linked immunoassays may be relatively straightforward because the labeling and immunoreaction procedures have been well developed for clinical time-resolved immunofluorometric assays.


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