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DOI: 10.1039/A800128F (Paper) Reference Section for: Analyst, 1998, 123, 1529-1533

Sensitive reversed-phase liquid chromatographic determination of fluoride based on its ternary systems with zirconium(IV) or hafnium(IV) and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

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Sławomir Oszwałdowski, Robert Lipka, Maciej Jarosz and Tadeusz Majewski

Abstract

Optimum conditions for the direct reversed-phase LC determination of fluoride based on the ternary M–F––(5-Br-PADAP) complexes [M = ZrIV or HfIV and 5-Br-PADAP = 2-(5-bromo-2-pyridylazo)- 5-diethylaminophenol] were evaluated. Chromatographic separation was performed with C18 end-capped column with an eluent consisting of acetonitrile–water (85 +15 v/v) mixture of pH 4.0 ± 0.3 (flow rate 1 ml min–1), and the eluate was monitored spectrophotometrically at λmax = 585 nm. The calibration curves were linear over a wide range of fluoride concentrations: from 1 to 110 and 150 ng ml–1 for the ZrIV–F––(5-Br-PADAP) and HfIV–F––(5-Br-PADAP) systems, respectively (using a 20 µl loop). Under such conditions the detection limits were 0.8 and 0.7 ng ml–1, respectively, and the quantification limit is 1.0 ng ml–1 for both methods. When a 100 µl loop was used, the limits of both detection and quantification in the method based on the zirconium system were 0.2 ng ml–1. Using the proposed method, fluoride was determined directly in tap water, saliva and an anti-cancer agent for prostatic cancer (Leuprolid).

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