Determination and Speciation of Arsenic in Human Urine by Ion-Exchange Chromatography/Flow Injection Analysis with Hydride Generation/Atomic Absorption Spectroscopy

1994 ◽  
Vol 77 (2) ◽  
pp. 441-445 ◽  
Author(s):  
O Jimenez de Blas ◽  
S Vicente Gonzalez ◽  
R Seisdedos Rodriguez ◽  
J Hernandez Mendez

Abstract A flow injection–hydride generation/atomic absorption spectroscopic method for the measurement of total urinary arsenic and for the selective determination of inorganic arsenic, monomethylarsonic acid (MMAA), and dimethylarsinic acid (DMAA) was developed. Destruction of the organic matrix is necessary to measure total arsenic content of urine samples. Digestion of this matrix with HNO3–H2SO4–H2O2 is described. The separation of inorganic, monomethylated, and dimethylated arsenic compounds in urine was performed with ion-exchange chromatography on AG 50 W-X8 resin. Detection limits of 2 ppb for each arsenic form and of 3 ppb for total arsenic in urine analyzed after mineralization were found. Recoveries in triplicate urine samples spiked with 10 ppb inorganic arsenic, 20 ppb MMAA, and 40 ppb DMAA were 93, 91, and 85%, respectively. The precision (relative standard deviation) of the method obtained in 10 replicate analyses of urine samples spiked with arsenic metabolites varied from 3.2 to 4.6%. This method is applicable to urine samples in studies relating to arsenic exposure and its monitoring.

1996 ◽  
Vol 79 (3) ◽  
pp. 764-768 ◽  
Author(s):  
Oroncio Jiménez De Blas ◽  
N Rodriguez Mateos ◽  
A Garcia Sanchez

Abstract A procedure has been developed for determination of total arsenic and selenium in soils and plants by atomic absorption spectrometry with hydride generation associated with flow injection analysis (FIA-AAS-HG). Samples were wet-digested by using 2 systems: heating in a metal digestion block with controlled temperature and time and heating in a microwave oven. Total arsenic and selenium were reduced with NaBH4 and concentrated HCI, respectively. In both digestion systems used for the 2 matrix types, detection limits below 1 μg/L were found for both elements for an injection volume of 160 μL, with relative standard deviations of 3–6%. Recoveries by the method ranged from 93 to 105%; with the reference materials FD8 and MRG-1, the values obtained in all cases were consistent with the certified data. The FIA-AAS-HG procedure is highly suitable for determination of total arsenic and selenium in soils and plants, and because of the coupled system used, it is an improvement over other procedures in terms of sample treatment, sample consumption, and automation.


2015 ◽  
Vol 69 (6) ◽  
Author(s):  
Hamid Shirkhanloo ◽  
Aisan Khaligh ◽  
Hassan Zavvar Mousavi ◽  
Mohammad Mehdi Eskandari ◽  
Ali Akbar Miran-Beigi

AbstractA simple, fast, and sensitive method for speciation and determination of As (III, V) and Hg (II, R) in human blood samples based on ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) and flow injection hydride generation/cold vapor atomic absorption spectrometry (FI-HG/CV-AAS) has been developed. Tetraethylthiuram disulfide, mixed ionic liquids (hydrophobic and hydrophilic ILs) and acetone were used in the DLLME step as the chelating agent, extraction and dispersive solvents, respectively. Using a microwave assisted-UV system, organic mercury (R-Hg) was converted to Hg(II) and total mercury amount was measured in blood samples by the presented method. Total arsenic content was determined by reducing As(V) to As(III) with potassium iodide and ascorbic acid in a hydrochloric acid solution. Finally, As(V) and R-Hg were determined by mathematically subtracting the As(III) and Hg(II) content from the total arsenic and mercury, respectively. Under optimum conditions, linear range and detection limit (3σ) of 0.1-5.0 μg L


1993 ◽  
Vol 39 (8) ◽  
pp. 1662-1667 ◽  
Author(s):  
C P Hanna ◽  
J F Tyson ◽  
S McIntosh

Abstract A method has been developed for the determination of inorganic arsenic [As(III) and As(V)] and its organic metabolites (monomethylarsenic and dimethylarsenic) in urine by flow-injection hydride generation atomic absorption spectrometry. The nontoxic seafood-derived arsenobetaine and arsenocholine species were first separated by a solid-phase extraction procedure. The remaining sample was digested with a mixture of nitric and sulfuric acids and potassium dichromate, followed by attack with hydrogen peroxide. The resulting As(V) was reduced to As(III) with potassium iodide in hydrochloric acid before injection into the flow-injection manifold. The percentage analytical recoveries (mean +/- 95% confidence interval) of various arsenic species added to a urine specimen at 250 micrograms/L were 108 +/- 2, 112 +/- 11, 104 +/- 7, and 95 +/- 5 for As(III), As(V), monomethylarsenic, and dimethylarsenic, respectively. For the determination of arsenic in Standard Reference Material 2670 (toxic metals in human urine), results agreed with the certified value (480 +/- 100 micrograms/L). Analyses of samples for the Centre de Toxicologie du Quebec, containing seafood-derived species, demonstrated the viability of the separation procedure. Detection limits were between 0.1 and 0.2 microgram/L in the solution injected into the manifold, and precision at 10 micrograms/L was between 2% and 3% (CV). These preliminary results show that the method might be applicable to determinations of arsenic in a range of clinical urine specimens.


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