Phthalate esters and phosphate esters in samples of indoor air from 27 houses in the Tokyo Metropolitan area were quantified using gas chromatograph/ mass spectrometer and gas chromatograph/flame photometric detector after adsorption on to charcoal and solvent extraction. The median concentrations of diethyl phthalate, dibutyl phthalate (DBP), butylbenzyl phthalate, dicyclohexyl phthalate and diethylhexyl phthalate were 0.10, 0.39, 0.01, 0.07 and 0.11 mg/m 3 , respectively. The median concentrations of tributyl phosphate, tris(2-chloroethyl) phosphate, triphenyl phosphate and tris(2-butoxyethyl) phosphate were less than 0.001 mg/m 3 . DBP was detected at the highest concentration (6.18 mg/m 3 ) in a new residential housing. This research indicated that exposure to phthalate esters through inhalation of air from the indoor environment is as important as dietary intake of phthalate esters, and can contribute to daily intake to a much greater extent than has been assumed hitherto.
The aim of this study was to assess the performance of a method of analyzing organic esters of plasticizer in indoor air by sampling air in a charcoal tube and extracting the esters in toluene using a gas chromatography-mass spectrometer (GC-MS) and flame photometric detector (FPD). An internal standardization method was used for the GC-MS measurement of phthalate esters, whereas an external calibration method was employed to determine the levels of phosphate esters by FPD. The instrumental detection limit, the instrumental lower limit of determination, and the blank and method detection limits were also determined. Mean recoveries of phthalate esters from the charcoal tube were 97.9-115%. Mean recoveries of phosphate esters were lower but reproducible. Recoveries of the esters from indoor air were generally greater than 80%. For all the compounds, no significant breakthrough was detected up to 100 microg. Thus, indoor organic esters could be accurately determined in the range of 0.6 x 10(-3)-23 microg/m3 by the procedure presented here. Preliminary analysis of the organic esters indicated that exposure to phthalate esters via indoor air inhalation could constitute a significant contribution to total daily intake.
Cadmium (Cd), lead (Pb), and selenium (Se) concentrations in cord whole blood, sampled from 24 women at the time of delivery in a hospital in Tokyo in 2005, were determined by inductively coupled plasma mass spectrometry with a reaction cell. Signal enhancement caused by nonspectroscopic interference for Se was evident and the standard addition technique was essential for correcting the interference. Median concentration in cord bloods was 0.20 ng/g, 6.7 ng/g (0.67 microg/dL), and 191 ng/g for Cd, Pb and Se, respectively. Lead concentration was lower, whereas Se concentration was higher, than those reported in other countries. The trace element concentration was related to the levels of thyroid stimulating hormone (TSH) and free thyroxin (fT4) in the neonatal blood sampled at 4-6 days postpartum. A significantly negative correlation was observed between Cd concentrations in cord blood and TSH concentration in neonatal blood. The result indicated the possible effect of in utero Cd exposure on thyroid hormone status of newborns and that Cd exposure level should be assessed as a covariate in the survey on the relationship between in utero chemicals (e.g., PCBs) exposure and thyroid hormone status.
A proficiency test for the analysis of pesticide residues in brown rice was carried out to support upgrading in analytical skills of participant laboratories. Brown rice containing three target pesticides (etofenprox, fenitrothion, and isoprothiolane) was used as the test samples. The test samples were distributed to the 57 participants and analyzed by appropriate analytical methods chosen by each participant. It was shown that there was no significant difference among the reported values obtained by different types of analytical method. The analytical results obtained by National Metrology Institute of Japan (NMIJ) were 3 % to 10 % greater than those obtained by participants. The results reported by the participant were evaluated by using two types of z-scores, that is, one was the score based on the consensus values calculated from the analytical results of participants, and the other one was the score based on the reference values obtained by NMIJ with high reliability. Acceptable z-scores based on the consensus values and NMIJ reference values were achieved by 87 % to 89 % and 79 % to 94 % of the participants, respectively.
Brown rice powder certified reference material, NMIJ CRM 7504-a, for the analysis of pesticide residues was developed by the National Metrology Institute of Japan, part of the National Institute of Advanced Industrial Science and Technology. Brown rice sample was harvested to contain the pesticides such as etofenprox and fenitrothion, and that was collected from a field in Ibaraki Prefecture in Japan. The certification was carried out using multiple analytical methods such as pressurized liquid extraction, homogenization, and solid-liquid extraction (shaking); the values of target pesticides were obtained by isotope dilution mass spectrometry. Certified values were 0.19 +/- 0.05 mg/kg and 0.109 +/- 0.017 mg/kg for etofenprox and fenitrothion, respectively.
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