Determination of chromium in urine samples by complexation–supercritical fluid extraction and liquid or gas chromatography

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 785; no. 2; pp. 303 - 309
• Main Authors: Arancibia, Veronica, Valderrama, Mauricio, Silva, Karina, Tapia, Tania
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 05.03.2003
• Subjects: Adult; Aged; Aged, 80 and over; Chromatography, Gas; Chromatography, High Pressure Liquid; Chromium; Chromium - urine; Complexation; Diabetes Mellitus - urine; Female; Humans; Indicators and Reagents; Male; Mass Spectrometry; Middle Aged; Pressure; Reference Standards; Reproducibility of Results; Solutions; Solvents; Spectrophotometry, Ultraviolet; Supercritical fluid extraction; Temperature; Chromium; Complexation; Supercritical fluid extraction
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/S1570-0232(02)00924-8

A method was developed for the determination of chromium as the Cr(acac) 3 complex in urine using SFE and chromatography. Quantitative extractions were achieved when the experiments were carried out under 3000 p.s.i. of pressure, at a temperature of 120 °C, with 2.0 ml of methanol, 30 min of static extraction and 5 min of dynamic extraction. The chromium was quantified by GC–FID detection. The calibration graph of Cr(acac) 3 solutions was linear between 0.50 and 43.0 μg ml −1 of chromium (DL 0.18 μg ml −1, R=0.9994). The same extracts were quantified by HPLC-340 nm detection. The calibration curve of the Cr(acac) 3 solutions was linear over a range of 0.013 to 60.0 μg ml −1 (DL 0.02 μg ml −1, R=0.9999). This method was applied to urine samples from 60 diabetic patients and 21 healthy volunteers. Chromium concentration ranges were 2.5–29.5 μg l −1 for the diabetics and 5.9–12.3 μg l −1 for the normal subjects.