Document Detail

Determination of Cd and Pb in food slurries by GFAAS using cryogenic grinding for sample preparation.
MedLine Citation:
PMID:  12043022     Owner:  NLM     Status:  MEDLINE    
A simple method combining slurry sampling after cryogenic grinding and the use of a permanent modification of the integrated platform inside the transversely heated graphite atomizer (THGA) was proposed for the determination of Cd and Pb in foods. Potentialities of the cryogenic grinding were evaluated for grinding different materials of difficult homogenization such as high fat and high fiber tissues. Animal and vegetal samples were cut into small pieces and ground in liquid nitrogen for 2 min. Slurries were prepared directly in the autosampler cup after cryogenic grinding by transferring an exact amount of homogeneous powdered material (5-20 mg) to the cup, followed by 1.00 mL of 0.2% (v/v) HNO3 containing 0.04% (v/v) Triton X-100 and sonication for 30 s, before transferring into the platform previously coated with 250 microg W and 200 microg Rh. Use of a tungsten carbide-rhodium permanent modifier combined with NH4H2PO4 conventional modifier improves tube lifetime and increases the pyrolysis temperature for Cd. Homogeneity tests, carried out by comparing the between- and within-batch precision for each kind of sample, showed no significant differences at the 95% confidence level, indicating good homogeneity for 5-20 mg masses. Detection limits were 3.3 ng g(-1) Cd and 75 ng g(-1) Pb for 1% m/v slurries. Results for determination of Cd and Pb in foods slurries were in agreement with those obtained with digested samples, since no statistical differences were found by the paired t-test at the 95% level.
D Santos; F Barbosa; A C Tomazelli; F J Krug; J A Nóbrega; M A Z Arruda
Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't     Date:  2002-05-04
Journal Detail:
Title:  Analytical and bioanalytical chemistry     Volume:  373     ISSN:  1618-2642     ISO Abbreviation:  Anal Bioanal Chem     Publication Date:  2002 Jun 
Date Detail:
Created Date:  2002-06-03     Completed Date:  2002-07-18     Revised Date:  2006-11-15    
Medline Journal Info:
Nlm Unique ID:  101134327     Medline TA:  Anal Bioanal Chem     Country:  Germany    
Other Details:
Languages:  eng     Pagination:  183-9     Citation Subset:  IM    
Centro de Energia Nuclear na Agricultura, USP-Caixa Postal 96, CEP: 13400-970, Piracicaba-SP, Brazil.
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MeSH Terms
Cadmium / analysis*
Food Analysis / methods*
Lead / analysis*
Spectrophotometry, Atomic / methods*
Reg. No./Substance:
7439-92-1/Lead; 7440-43-9/Cadmium

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