TY - JOUR
T1 - Development of analytical method for determination of Sb(V), Sb(III) and TMSb(V) in occupationally exposed human urine samples by HPLC-HG-AFS
AU - Quiroz, Waldo
AU - Arias, Helen
AU - Bravo, Manuel
AU - Pinto, Marcela
AU - Lobos, María Gabriela
AU - Cortés, Marisol
N1 - Funding Information:
The authors gratefully acknowledge the financial support of FONDECYT (project 11080084 ). We especially thank our teachers Dr. Ida De Gregori and Dr. Hugo Pinochet for the high quality science education that they gave us and we wish them a happy retirement.
PY - 2011/1
Y1 - 2011/1
N2 - In the present paper, we develop a methodology for antimony speciation in occupationally exposed human urine samples by high-performance liquid chromatography with hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS). The methodology was applied to the determination of Sb(V), Sb(III) and (CH3)3SbCl2 (TMSb(V)). Retention time of Sb(V), Sb(III) and TMSb(V) species were 0.88, 2.00 and 3.61 and the detection limits were 0.18, 0.19 and 0.12μg L-1, for 100μL loop injection respectively which is considered useful for elevated/occupationally exposed urine samples. Studies on the stability of antimony species in urine samples on the function of the elapsed time of preservation (4°C) and storage (-70°C) were performed. Results revealed that antimony species are highly unstable at -70°C, probably due to co-precipitation reaction. In this kind of matrix transformation during preservation time may occur, such as oxidation of Sb(III) to Sb(V) and transformation into species that do not elute from the column. EDTA shows that it is able to stabilize Sb(III) for more than one week of preservation time at 4°C avoiding co-precipitation during storage at -70°C. Finally the methodology was applied to occupationally exposed human urine samples. 25% of specimens present antimony levels (Sb(V)) of more than 5μg L-1.
AB - In the present paper, we develop a methodology for antimony speciation in occupationally exposed human urine samples by high-performance liquid chromatography with hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS). The methodology was applied to the determination of Sb(V), Sb(III) and (CH3)3SbCl2 (TMSb(V)). Retention time of Sb(V), Sb(III) and TMSb(V) species were 0.88, 2.00 and 3.61 and the detection limits were 0.18, 0.19 and 0.12μg L-1, for 100μL loop injection respectively which is considered useful for elevated/occupationally exposed urine samples. Studies on the stability of antimony species in urine samples on the function of the elapsed time of preservation (4°C) and storage (-70°C) were performed. Results revealed that antimony species are highly unstable at -70°C, probably due to co-precipitation reaction. In this kind of matrix transformation during preservation time may occur, such as oxidation of Sb(III) to Sb(V) and transformation into species that do not elute from the column. EDTA shows that it is able to stabilize Sb(III) for more than one week of preservation time at 4°C avoiding co-precipitation during storage at -70°C. Finally the methodology was applied to occupationally exposed human urine samples. 25% of specimens present antimony levels (Sb(V)) of more than 5μg L-1.
KW - Antimony speciation
KW - HPLC-HG-AFS
KW - Urine
UR - http://www.scopus.com/inward/record.url?scp=78649635701&partnerID=8YFLogxK
U2 - 10.1016/j.microc.2010.06.015
DO - 10.1016/j.microc.2010.06.015
M3 - Article
AN - SCOPUS:78649635701
VL - 97
SP - 78
EP - 84
JO - Microchemical Journal
JF - Microchemical Journal
SN - 0026-265X
IS - 1
ER -