Philippeit G, Angerer J
Institute and Outpatient Clinic of Occupational-, Social- and Environmental Medicine, Friedrich-Alexander-Universität, Erlangen, Germany.
J Chromatogr B Biomed Sci Appl. 2001 Sep 5;760(2):237-45. doi: 10.1016/s0378-4347(01)00271-7.
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.
下述采用紫外检测的高效液相色谱法可选择性测定人尿中的痕量钯。经紫外光解破坏全部有机基质后，通过固相萃取（SPE）对钯进行选择性富集。反相C18固相萃取柱材料装填有配体N，N - 二乙基 - N'-苯甲酰基硫脲（DEBT），该配体在酸性溶液及室温下对钯具有出色的络合能力。用乙醇洗脱Pd(DEBT)₂络合物。在分析柱上进行等度分离（甲醇/水98:2（v/v））后，于274 nm处检测该络合物。检测限为10 ng Pd/l。同组内不精密度的相对标准偏差（RSD）在11%（75 ng Pd/l）至7%（180 ng Pd/l）范围内。日间不精密度为11%（75 ng Pd/l）和5%（180 ng Pd/l）。回收率在94%至96%之间。使用该方法分析了44名普通人群的尿样。仅在一份尿样中检测到钯。作为对比，对10名有职业性钯暴露的人员进行了检查。尿中浓度范围为<10至2538 ng/l。
