scholarly journals High-Throughput Determination of Seven Trace Elements in Food Samples by Inductively Coupled PlasmaMass Spectrometry

2006 ◽  
Vol 89 (2) ◽  
pp. 469-479 ◽  
Author(s):  
Kwok Chu Chan ◽  
Yiu Chung Yip ◽  
Hei Shing Chu ◽  
Wing Cheong Sham
Keyword(s):  
High Throughput ◽  
Interlaboratory Comparison ◽  
Certified Reference Materials ◽  
Food Samples ◽  
Inductively Coupled ◽  
Microwave Assisted ◽  
Z Scores ◽  
Sample Dilution ◽  
Microwave Assisted Digestion

Abstract A method was developed for high-throughput determinations of 7 elements in food samples, namely antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), and tin (Sn). The samples were digested by closed-vessel microwave-assisted digestion using concentrated nitric acid (HNO3) as the medium, followed by microwave- assisted evaporation to concentrate the sample solutions before dilution to the desired volume. The microwave-assisted evaporation procedure effectively reduced the final acid concentration to around 8 before analysis by inductively coupled plasmamass spectrometry (ICPMS). This reduction allows determination by ICPMS to proceed without further sample dilution, which would affect the detection limit. The method was validated, and method recoveries for As, Cd, Cr, Pb, and Hg were within the certified ranges of the chosen certified reference materials. Recoveries of the 7 elements from spiked samples ranged from 93.1 to 103.6. The standard uncertainties of precision for the 7 elements were between 3.1 and 4.3. Interlaboratory comparison studies for As, Cd, and Pb gave z-scores ranging from 0.2 to 0.3.

scholarly journals Inductively Coupled Plasma Collision Cell Quadrupole Mass Spectrometric Determination of Extractible Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave-Assisted Digestion: Results from an FDA Interlaboratory Study

2019 ◽  
Vol 102 (2) ◽  
pp. 590-604 ◽  
Author(s):  
Patrick J Gray ◽  
William Cunningham
Keyword(s):  
Inductively Coupled Plasma ◽  
Mass Spectrometric ◽  
Interlaboratory Study ◽  
Standard Reference Materials ◽  
Inductively Coupled ◽  
Microwave Assisted ◽  
Mass Spectrometric Determination ◽  
Microwave Assisted Digestion ◽  
Better Than

Abstract Background: An interlaboratory study was conducted to test U.S. Food and Drug Administration (FDA) Elemental Analysis Manual (EAM) Method 4.7, “Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion.” Objective: The goal of the study was to demonstrate the performance of FDA EAM Method 4.7. Methods: Fourteen laboratories participated in the collaborative study, including nine Food Emergency Response Network state laboratories and five federal FDA laboratories. Laboratories tested 8 labeled standard reference materials and 12 blinded foods: mayonnaise, dark chocolate, sunflowerseeds, hamburger with cheese, brown rice flour (blinded reference material included as a test food), infant formula, canned smoked oysters, sardines in tomato paste, swordfish, mineral water, cinnamon, and a multivitamin. The blinded test foods represented every sector of the AOAC food triangle. Participants measured the mass fraction of each element in each sample in triplicate. Results:Horwitz Ratio (HorRat) values were better than 1.5 for all As, Cd, Cu, Hg, Mo, Ni, Pb,and Se measurements when at least eight laboratories reported results greater than LOQ. The HorRat values were better than 1.5 for all Mn and Zn measurements except for the multivitamin and for all Cr measurements exceptfor sunflower seeds, in which the nonhomogeneity was identified. The average HorRat value of the blinded test foods was 0.66 for results greater than LOQ(n = 4206). Conclusions: The study showed that the method performed satisfactorily as a standard method for extractibleelemental analysis of food. Highlights: The method met or exceeded the performance expected.

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