Sensitive determination of fluoride in biological samples by gas chromatography–mass spectrometry after derivatization with 2-(bromomethyl)naphthalene
2014
Kwon, Sun-Myung | Shin, Ho-Sang
A gas chromatography–mass spectrometric method was developed in this study in order to determine fluoride in plasma and urine after derivatization with 2-(bromomethyl)naphthalene. 2-Fluoronaphthalene was chosen as the internal standard. The derivatization of fluoride was performed in the biological sample and the best reaction conditions (10.0mgmL−1 of 2-(bromomethyl)naphthalene, 1.0mgmL−1 of 15-crown-5-ether as a phase transfer catalyst, pH of 7.0, reaction temperature of 70°C, and heating time of 70min) were established. The organic derivative was extracted with dichloromethane and then measured by a gas chromatography–mass spectrometry. Under the established condition, the detection limits were 11μgL−1 and 7μgL−1 by using 0.2mL of plasma or urine, respectively. The accuracy was in a range of 100.8–107.6%, and the precision of the assay was less than 4.3% in plasma or urine. Fluoride was detected in a concentration range of 0.12–0.53mgL−1 in six urine samples after intake of natural mineral water containing 0.7mgL−1 of fluoride.
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