RESUMO
Systemic uptake of perchlorate anion, a rocket fuel component and potential thyroid function disruptor, by leafy vegetables and other crops grown in contaminated waters is a public health concern. A column-switching anion-exchange chromatographic method with suppressed conductivity detection, described in this paper, achieved a 3-6 microg/kg method limit of quantitation in analysis of the wet weight edible portion of cantaloupe, carrots, lettuce, and spinach samples with field-incurred perchlorate. A test portion was blended with dilute nitric acid, and the extract was filtered under vacuum. A portion of the measured filtrate was acidified to pH approximately 2 by addition of cation-exchange resin, 4 mL was passed through a graphitized carbon cleanup column, and an aliquot of a collected fraction was pushed through a short precolumn for anion extraction, enrichment, and injection onto the analytical column. Statistical comparison with determination by tandem mass spectrometry-ion chromatography analysis of untreated filtrate revealed that the difference between means was not significant at the 95% confidence level (P value > or = 0.12) for crops tested. In addition, the method was applied to cooked vegetables processed as baby food.
Assuntos
Cromatografia por Troca Iônica/métodos , Análise de Alimentos/métodos , Percloratos/análise , Cucumis melo/química , Daucus carota/química , Frutas/química , Temperatura Alta , Humanos , Lactente , Alimentos Infantis/análise , Lactuca/químicaRESUMO
A rapid, sensitive, and specific method was developed for determining perchlorate anion in lettuce, cantaloupe, bottled water, and milk. A test portion of chopped crop homogenate was extracted with diluted nitric acid and filtered. Milk proteins were precipitated with acetonitrile, and the supernatant, after centrifugation, was cleaned up on a graphitized carbon solid-phase extraction column. Water samples were analyzed directly. All test solutions were syringe filtered and mixed with an 18O4-labeled perchlorate internal standard before ion chromatography-tandem mass spectrometry. A strong anion exchange column eluted with 100 mM ammonium acetate in 50:50 (v/v) acetonitrile/water was interfaced via electrospray ionization to a triple stage quadrupole mass spectrometer operated in the negative ion mode. The labeled internal standard corrected for any sample matrix effects on measured signals. Four parent-to-product ion transitions, for loss of oxygen, were monitored for native and 18O4-labeled perchlorate anion, respectively: 35Cl-perchlorate, m/z 99 --> 83 and 107 --> 89; 37Cl-perchlorate, m/z 101 --> 85 and 109 --> 91. The limit of quantitation was 1.0 microg/kg in lettuce, 2.0 microg/kg in cantaloupe, 0.50 microg/L in bottled water, and 3.0 microg/L in milk. Native perchlorate was recovered from fortified test portions in the range 93-107% for lettuce, 107-114% for cantaloupe, 100-115% for bottled water, and 99-101% for milk.
Assuntos
Cromatografia por Troca Iônica/métodos , Análise de Alimentos/métodos , Espectrometria de Massas/métodos , Percloratos/análise , Percloratos/química , Animais , Bovinos , Cucumis melo/química , Lactuca/química , Leite/química , Sensibilidade e Especificidade , Água/químicaRESUMO
The arsenic, cadmium, mercury, and lead contents of 95 dietary supplement products were determined using microwave digestion and high-resolution inductively coupled plasma mass spectrometry. Precision and accuracy were demonstrated by element recovery from 17 dietary supplements and replicates of 8 reference materials. The concentration ranges were as follows: arsenic, <5-3770 microg/kg; cadmium, <10-368 microg/kg; mercury, <80-16800 microg/kg; and lead, <20-48600 microg/kg. An assessment of estimated exposures/intakes of the four elements is presented.