Assessment of tropane alkaloid levels in Brazilian buckwheat flour products: A novel LC-UHPLC-MS/MS approach using solid-liquid extraction at low temperature.

In recent years, the monitoring of tropane alkaloids, specifically hyoscyamine and scopolamine, in food has become a pressing concern. This is due to increasing reports of food contamination with these compounds worldwide, raising awareness about the potential risks associated with their consumption. A novel method is proposed here for the determination of the sum of (+)-hyoscyamine, (-)-hyoscyamine, and (-)-scopolamine in buckwheat-based matrices, using solid-liquid extraction at low temperature and quantification by bidimensional chromatography coupled to tandem mass spectrometry. The validated method presented a linear response in the concentration range of 2.5-15 µg kg-1 (r > 0.99). The precision and accuracy were in the ranges from 0.8 to 11.0 % and from 96 to 103 %, respectively. The limit of quantification (LOQ) was 2.5 µg kg-1. No contamination was found at levels above the LOQ in any of the 18 samples analyzed (buckwheat flour, grains, and gluten-free mix).

Bee pollen as a bioindicator of environmental pesticide contamination.

Honeybees and bee products are potential bioindicators of the presence of contaminants in the environment, enabling monitoring of large areas due to the long distances travelled by bees. This work evaluates the use of bee pollen as a bioindicator of environmental contamination by pesticides. A GC-MS/MS analytical method for multiresidue determination of 26 different pesticides in pollen was developed and validated in accordance with the recommendations of the European Union SANCO guide. Environmental monitoring was conducted using the analysis of 145 pollen samples collected from ten beehives in the experimental apiary of Embrapa in Jaguariúna (São Paulo State, Brazil). Bioallethrin and pendimethalin were identified in four and eighteen samples, respectively, at concentrations below the LOQ of the method (25 ng g(-1)). Passive sampling with polyurethane foam discs was used as a control, and no pesticides were found. The detection of pesticide residues in seven samples (33%) from commercial apiaries in Ribeirão Preto (São Paulo State) confirmed the efficiency of the analytical method and the need for environmental monitoring for the presence of pesticide residues. The results demonstrated the potential of bee pollen as a bioindicator of environmental contamination by pesticides.

Development of an analytical method for the quantification of pfaffic acid in Brazilian ginseng (Hebanthe eriantha).

Hebanthe eriantha (Poir.) Pedersen (Amaranthaceae), which is known as Brazilian ginseng is widely used in folk medicine as an aphrodisiac and antidiabetic tonic. The anti-tumor activity, attributed to the pfaffic acid present in roots of H. eriantha, is responsible for the great interest in the commercialization of this species. In Brazil, the species H. eriantha is mainly used in commercial preparations, although other plants of the genus Pfaffia and Hebanthe have been marketed as Pfaffia paniculata or Brazilian ginseng. The pfaffic acid present in the roots is mainly conjugated with sugars (pfaffosides) and can be used as an active marker of H. eriantha, which helps to differentiate this species from others marketed as Brazilian ginseng. The main objective of this study was to develop and validate a liquid chromatographic method to quantify pfaffic acid in the roots of H. eriantha. The extraction and hydrolysis conditions were optimized using an univariate and experimental design, respectively, and the quantification of pfaffic acid by high performance liquid chromatography with diode-array detection (HPLC-DAD) was validated. This method was used to evaluate the pfaffic acid content in 30 different genotypes of the species from a germplasm collection. The content of pfaffic acid ranged from 0.97 to 4.29% (w/w) on a dry weight basis.

Simultaneous determination of cadmium and lead in medicinal plants by anodic stripping voltammetry.

A simple method for the simultaneous determination of Cd and Pb in medicinal plants by differential pulse anodic stripping voltammetry, using a hanging mercury drop electrode, was developed. The pre-concentration of the metals was performed in 0.8 mol L(-1) HCl at -0.73V for 180s. The sample preparation was carried out by dry-ashing 1.0g of finely pulverized plant samples for 2.5h at 500 degrees C. The determination limit of the method was 0.12 and 0.010 mg kg(-1) for Pb and Cd, respectively. The method was applied to the quantification of cadmium and lead in samples of Hypericum perforatum, Mikania guaco, Mikania glomerata and Peamus boldus. The voltammetric method was shown to be useful for the control of contaminants in medicinal plants.