Determination of palladium in human urine by high-performance liquid chromatography and ultraviolet detection after ultraviolet photolysis and selective solid-phase extraction. 2001

G Philippeit, and J Angerer
Institute and Outpatient Clinic of Occupational-, Social- and Environmental Medicine, Friedrich-Alexander-Universität, Erlangen, Germany.

The high-performance liquid chromatographic method with UV detection described below permits the selective determination of traces of palladium in human urine. After UV photolysis, during which the complete organic matrix was destroyed, the palladium was selectively enriched by solid-phase extraction (SPE). The reversed-phase C18 SPE column material was loaded with the ligand N,N-diethyl-N'-benzoylthiourea (DEBT) which shows an excellent complexing capacity for palladium in acidic solutions and at room temperature. The Pd(DEBT)2 complex was eluted with ethanol. After isocratic separation on the analytical column (MeOH/H2O 98:2 (v/v)), the complex was detected at 274 nm. The detection limit was 10 ng Pd/l. The relative standard deviations (RSD) of the within-series imprecision were in the range between 11% (75 ng Pd/l) and 7% (180 ng Pd/l). The between-day imprecision was 11% (75 ng Pd/l) and 5% (180 ng Pd/l). The recovery rates ranged between 94 and 96%. Using this method, urine samples of 44 persons from the general population were analysed. Only in one urine sample could palladium be detected. For comparison, 10 persons with occupational palladium exposure were examined. The urinary concentrations ranged from <10 to 2,538 ng/l.

UI MeSH Term Description Entries
D008297 Male Males
D010165 Palladium A chemical element having an atomic weight of 106.4, atomic number of 46, and the symbol Pd. It is a white, ductile metal resembling platinum, and following it in abundance and importance of applications. It is used in dentistry in the form of gold, silver, and copper alloys.
D010777 Photochemistry A branch of physical chemistry which studies chemical reactions, isomerization and physical behavior that may occur under the influence of visible and/or ultraviolet light. Photochemistries
D002138 Calibration Determination, by measurement or comparison with a standard, of the correct value of each scale reading on a meter or other measuring instrument; or determination of the settings of a control device that correspond to particular values of voltage, current, frequency or other output. Calibrations
D002851 Chromatography, High Pressure Liquid Liquid chromatographic techniques which feature high inlet pressures, high sensitivity, and high speed. Chromatography, High Performance Liquid,Chromatography, High Speed Liquid,Chromatography, Liquid, High Pressure,HPLC,High Performance Liquid Chromatography,High-Performance Liquid Chromatography,UPLC,Ultra Performance Liquid Chromatography,Chromatography, High-Performance Liquid,High-Performance Liquid Chromatographies,Liquid Chromatography, High-Performance
D005260 Female Females
D006801 Humans Members of the species Homo sapiens. Homo sapiens,Man (Taxonomy),Human,Man, Modern,Modern Man
D012680 Sensitivity and Specificity Binary classification measures to assess test results. Sensitivity or recall rate is the proportion of true positives. Specificity is the probability of correctly determining the absence of a condition. (From Last, Dictionary of Epidemiology, 2d ed) Specificity,Sensitivity,Specificity and Sensitivity
D013056 Spectrophotometry, Ultraviolet Determination of the spectra of ultraviolet absorption by specific molecules in gases or liquids, for example Cl2, SO2, NO2, CS2, ozone, mercury vapor, and various unsaturated compounds. (McGraw-Hill Dictionary of Scientific and Technical Terms, 4th ed) Ultraviolet Spectrophotometry
D014466 Ultraviolet Rays That portion of the electromagnetic spectrum immediately below the visible range and extending into the x-ray frequencies. The longer wavelengths (near-UV or biotic or vital rays) are necessary for the endogenous synthesis of vitamin D and are also called antirachitic rays; the shorter, ionizing wavelengths (far-UV or abiotic or extravital rays) are viricidal, bactericidal, mutagenic, and carcinogenic and are used as disinfectants. Actinic Rays,Black Light, Ultraviolet,UV Light,UV Radiation,Ultra-Violet Rays,Ultraviolet Light,Ultraviolet Radiation,Actinic Ray,Light, UV,Light, Ultraviolet,Radiation, UV,Radiation, Ultraviolet,Ray, Actinic,Ray, Ultra-Violet,Ray, Ultraviolet,Ultra Violet Rays,Ultra-Violet Ray,Ultraviolet Black Light,Ultraviolet Black Lights,Ultraviolet Radiations,Ultraviolet Ray

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