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Ammonium acetate is employed in order to develop a novel HPLC-ICP-MS arsenic speciation methodology applicable to six arsenic species, i.e, AC, AB, As III , As V , DMA and MMA. The most predominant species in the toxicological field are covered in a 30-min chromatogram with reproducible and repeatability peak area ratio. Moreover, typical problems from traditional methods are sorted out by using a robust, high-selective and 75 ArCl + interference-free methodology. Chromatographic and detector optimization ensures low LOQs for each species with acceptable precision and accuracy values obtained using four urinary arsenic speciation PTS enabling to be useful for sub ng mL -1 arsenic exposure assessments., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Background: Very few studies exist on urinary arsenic exposure in Spain., Objective: To evaluate total and speciated urinary arsenic (As) levels in a Spanish population sample., Methods: Demographic, lifestyle and dietary data was collected for 124 volunteers (aged 20-76years; 88 women and 36 men), who were tested for total arsenic and five arsenic species using high-performance liquid chromatography-inductively coupled plasma mass spectrometry., Results: Arsenobetaine (AB) and dimethylarsinic acid (DMA) were detected in 96.8% of the study participants (limit of detection (LOD) 1.0μg/L for AB and 1.9μg/L for DMA). Monomethylarsonic acid (MMA) and arsenous acid (As(III)) were detected in 5.6% (LOD 1.8μg/L) and 1.6% (LOD 1.4μg/L) of the participants, respectively; arsenic acid (As(V)) was not detected (LOD 1.4μg/L). AB and DMA (geometric mean (GM) 29.1μg/L and 7.5μg/L, respectively) were the main contributors to total urinary arsenic levels. Urinary DMA was positively associated with AB., Conclusion: Total arsenic levels observed in the Spanish population sample were higher than those reported by other European studies. The most recurrent urinary arsenic species was AB, followed by DMA, probably attributable to the high Spanish consumption of seafood. We recommend using inorganic As+MMA as the two main urinary biomarkers for inorganic As exposure. Our results provide reference data for analysing arsenic speciation results and assessing human exposure., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Objective: The aim of this report is to propose a scheme for validation of an analytical technique according to ISO 17025., Material and Methods: According to ISO 17025, the fundamental parameters tested were: selectivity, calibration model, precision, accuracy, uncertainty of measurement, and analytical interference., Results: A protocol has been developed that has been applied successfully to quantify zinc in serum by atomic absorption spectrometry., Conclusion: It is demonstrated that our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics., (Copyright © 2015 SECA. Published by Elsevier Espana. All rights reserved.)

This study analyzed the variation and relationship of several trace elements, metabolic substrates and stress hormones activated by exercise during incremental exercise. Seventeen well-trained endurance athletes performed a cycle ergometer test: after a warm-up of 10 min at 2.0 W kg(-1), the workload was increased by 0.5 W kg(-1) every 10 min until exhaustion. Prior diet, activity patterns, and levels of exercise training were controlled, and tests timed to minimize variations due to the circadian rhythm. Oxygen uptake, blood lactate concentration, plasma ions (Zn, Se, Mn and Co), serum glucose, non-esterified fatty acids (NEFAs) and several hormones were measured at rest, at the end of each stage and 3, 5 and 7 min post-exercise. Urine specific gravity was measured before and after the test, and participants drank water ad libitum. Significant differences were found in plasma Zn and Se levels as a function of exercise intensity. Zn was significantly correlated with epinephrine, norepinephrine and cortisol (r = 0.884, P < 0.01; r = 0.871, P < 0.01; and r = 0.808, P = 0.05); and Se showed significant positive correlations whit epinephrine and cortisol (r = 0.743, P < 0.05; and r = 0.776, P < 0.05). Neither Zn nor Se levels were associated with insulin or glucagon, and neither Mn nor Co levels were associated with any of the hormones or substrate metabolites studied. Further, while Zn levels were found to be associated only with lactate, plasma Se was significantly correlated with lactate and glucose (respectively for Zn: r = 0.891, P < 0.01; and for Se: r = 0.743, P < 0.05; r = 0.831, P < 0.05). In conclusion, our data suggest that there is a positive correlation between the increases in plasma Zn or Se and stress hormones variations induced by exercise along different submaximal intensities in well-hydrated well-trained endurance athletes., (Copyright © 2015 Elsevier GmbH. All rights reserved.)

The purpose of this study was to assess the effect of exercise intensity during an incremental exercise test on plasma Mg concentration in well-trained euhydrated athletes. Twenty-seven well-trained endurance athletes carried out a cycloergometer test: after a warm-up of 10 min at 2.0 W·kg(-1), the workload increased by 0.5 W·kg(-1) every 10 min until exhaustion. Oxygen uptake (VO(2)), blood lactate concentration ([La(-)](b)), catecholamines, and plasma Mg were measured at rest, at the end of each stage and at 3, 5 and 7 minutes post-exercise. Urine specific gravity (U(SG)) was analyzed before and after the test, and subjects drank water ad libitum. Fat oxidation rate (FAT(oxr)), carbohydrate oxidation rate (CHO(oxr)), energy expenditure from fat (EE(FAT)), energy expenditure from carbohydrate (EE(CHO)), and total EE (EE(TOTAL)) were estimated using stoichiometric equations. Plasma Mg concentration at each relative exercise intensity (W·kg(-1)) were compared by means of repeated-measures ANOVA. Pearson's correlations were performed to assess the relationship between variables. The significance level was set at p<0.05. No significant differences were found in U(SG) between before and after the test (1.014±0.004 vs 1.014±0.004 g·cm(-3)). Nor were significant differences found in plasma Mg as a function of the different exercise intensities. Further, no significant correlations were detected between Mg and metabolic variables. In conclusion, acute exercise at a range of submaximal intensities in euhydrated well-trained endurance athletes does not affect plasma Mg concentration, suggesting that the plasma volume plays an important role in Mg homeostasis during exercise.

The purpose of this study was to assess the effect of relative exercise intensity on various plasma trace elements in euhydrated endurance athletes. Twenty-seven well-trained endurance athletes performed a cycloergometer test: after a warm-up of 10 min at 2.0 W kg⁻¹, workload increased by 0.5 W kg⁻¹ every 10 min until exhaustion. Oxygen uptake, blood lactate concentration ([La⁻](b)), and plasma ions (Zn, Se, Mn and Co) were measured at rest, at the end of each stage, and 3, 5 and 7 min post-exercise. Urine specific gravity (U(SG)) was measured before and after the test, and subjects drank water ad libitum. Fat oxidation (FAT(OXR)), carbohydrate oxidation (CHO(OXR)), energy expenditure from fat (EE(FAT)), from carbohydrates (EE(CHO)) and total EE (EE(T)) were estimated using stoichiometric equations. A repeated measure (ANOVA) was used to compare plasma ion levels at each exercise intensity level. The significance level was set at P<0.05. No significant differences were found in U(SG) between, before, and after the test (1.014±0.004 vs. 1.014±0.004 g cm⁻³) or in any plasma ion level as a function of intensity. There were weak significant correlations of Zn (r=0.332, P<0.001) and Se (r=0.242, P<0.01) with [La⁻](b), but no relationships were established between [La⁻](b), VO₂, FAT(OXR), CHO(OXR), EE(FAT), EE(CHO), or EE(T) and plasma ion levels. Acute exercise at different submaximal intensities in euhydrated well-trained endurance athletes does not provoke a change in plasma trace element levels, suggesting that plasma volume plays an important role in the homeostasis of these elements during exercise., (Copyright © 2010 Elsevier GmbH. All rights reserved.)