Microwave-assisted digestion using dilute nitric acid solution and investigation of calibration strategies for determination of As, Cd, Hg and Pb in dietary supplements using ICP-MS.

This study proposes an analytical procedure for microwave-assisted sample preparation of dietary supplements for athletes using dilute nitric acid solution followed by determination of elemental impurities (As, Cd, Hg and Pb) by inductively coupled plasma mass spectrometry (ICP-MS) according to the United States Pharmacopeia Chapters 2232 and 233. Calibration strategies as internal standardization (IS), multi-isotope calibration (MICal), and one-point standard addition (OP SA) were applied for correction of matrix effects. The optimization of the sample preparation procedure was performed using Doehlert experimental design based on overall desirability results (residual acidity, dissolved organic carbon and recoveries reached for certified reference material of Typical Diet) for each calibration method evaluated. Accuracy was also evaluated by recovery experiments according to the permissible daily exposure specific for each element and samples were spiked with element concentrations of 0.5J and 1.5J in order to check accuracies for As, Cd, Hg and Pb. Recoveries ranged from 82 to 120% using IS, 90 to 125% using MICal, 88 to 120% using OP SA and the repeatability was demonstrated by a precision lower than 10% RSD. Ten samples of dietary sport supplements were analyzed using the three calibration methods evaluated and the concentrations of As, Cd and Pb determined in eight samples were lower than the limits established by the Chapter 2232.

Physiological responses of Chlorella sorokiniana to copper nanoparticles.

Copper (Cu) nanomaterials have been increasingly researched and produced for many different consumer products. They have high reactivity and bactericidal properties, making them important in antifouling paints, which are thus directly introduced into aquatic ecosystems. However, studies are scarce on the behavior of Cu nanoparticles (Cu-NPs) in natural aquatic systems and their interactions with primary producers such as microalgae. We investigated the effects of NPs on some physiological responses of the freshwater phytoplankton Chlorella sorokiniana. The cells were exposed to nominal concentrations ranging from 2.50 to 635.00 µg L-1 Cu-NPs for 96 h under laboratory-controlled conditions. The cultures were monitored daily for population growth and maximum photosynthetic quantum yield. Total lipids, proteins, and carbohydrates were quantified at 72 h of Cu-NP exposure. The results showed a positive correlation between nominal Cu-NPs and Cu in the biomass (0.97 correlation coefficient) and that this was inversely proportional to total carbohydrates, with a -0.64 correlation coefficient. At the higher end of the Cu-NP concentrations tested, higher total proteins and reduced growth rates were obtained in comparison with controls; we suggest that metal-binding proteins/antioxidants and nonstructural proteins were preferentially produced under these conditions. Our results contribute to an understanding of the interaction between Cu-NPs and a cosmopolitan phytoplankton, C. sorokiniana, and we emphasize that the disposal and use of Cu-NPs requires monitoring because even at environmentally relevant concentrations, the composition of the algae was affected. Environ Toxicol Chem 2019;38:387-395. © 2018 SETAC.

Direct analysis of deodorants for determination of metals by inductively coupled plasma optical emission spectrometry.

A fast and simple dilute-and-shoot procedure for determination of Al, As, Ba, Cd, Cu, Fe, Mg, Mn, Ni, Pb, Sc, Ti, V, Zn and Zr in deodorants by inductively coupled plasma optical emission spectrometry (ICP OES) was developed. Sample preparation was carried out by diluting 1 mL of deodorant sample in 1% (v v-1) HNO3. The accuracy of the analytical procedure was evaluated using addition and recovery experiments, and recoveries ranged from 80 to 119%. The limits of detection varied from 0.001 to 0.76 mg kg-1. Nine deodorants samples of different brands were analyzed. The maximum concentrations found (mg kg-1) were: Fe (1.0), Mn (0.1), Ti (1.02), V (0.33), Zn (255.2) and Zr (0.5); for Al and Mg, determined concentrations varied from 0.01 to 7.0% and from 0.005 to 1.44 mg kg-1, respectively, showing wide variation depending on the sample type. The developed procedure was adequate for determining these analytes in routine analysis presenting high sample throughput and demonstrated the feasibility of direct analysis measurements after simple dilution step.

Tungsten permanent chemical modifier for fast estimation of Se contents in soil by graphite furnace atomic absorption spectrometry.

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L(-1)) plus ammonium hydrogencarbonate (1.0 mol L(-1)) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degrees C assisted by air during 30 s. For 20 microL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 microgram of L(-1)) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was approximately 63 pg of Se, and the lifetime of the tube was approximately 750 firings. The limit of detection was 1.6 microgram L(-1), and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 microgram of L(-1). The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.