Separation of sugar isomers extracted from biological samples is challenging because of their natural occurrence as alpha and beta anomers and, in the case of hexoses, in their pyranose and furanose forms. A reductive amination method was developed for the tagging of sugars with the aim of it becoming part of a metabolomics work flow. The best separation of the common hexoses (glucose, fructose, mannose and galactose) was achieved when H-aniline was used as the tagging reagent in combination with separation on a ZICHILIC column. The method was used to tag a range of sugars including pentoses and uronic acids. The method was simple to perform and was able to improve both the separation of sugars and their response to electrospray ionisation. The method was applied to the profiling of sugars in urine where a number of hexose and pentose isomers could be observed. It was also applied to the quantification of sugars in post-mortem brain samples from three control samples and three samples from individuals who had suffered from bipolar disorder.
Using microwave technique in the presence of citric acid, selenium nanoparticles (SeNPs) were fabricated. The morphological characteristics revealed that the spherical SeNPs with diameters ranging from 10.5 to 20 nm aggregated spherical shapes with sizes ranging from 0.67 to 0.83 mm. Moreover, the antioxidant efficacy was assessed by the DPPH radical scavenging test, which depicted that green-prepared nanoparticle at a 106.3 mg/mL dosage had the maximum scavenging capacity (301.1 ± 11.42 mg/g). Otherwise, with nanoparticle concentrations of 500 mg/ml, in vitro cell viability of SeNPs through human breast cancer MCF-7 cell lines was reduced to 61.2 ± 2.2% after 1 day of exposure. The antibacterial activity was tested against G-negative
Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli
(
E. coli
), G-positive bacteria
Bacillus subtilis (B. subtilis)
,
and Staphylococcus aureus
(
S. aureus
), which demonstrated that SeNPs had little activity against
S. aureus
. Still, it had the highest activity against
E. coli
, with a zone of inhibition (ZOI) of 25.2 ± 1.5 mm compared to 16.0 ± 0.6 mm for the standard antibiotic. Most notably, biogenic SeNPs have anticoagulant activities using activated partial thromboplastin time (aPTT) assessment. Based on previous findings, SeNPs can be used in medical aid and their cell viability, antioxidant, anticoagulant, and effects on bacteria.
In the last decade, high-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) combined with electrospray ionization (ESI) has been widely used for determining low concentrations of steroids, and derivatization has often been employed to enhance detection. In the present study, endogenous steroids were extracted using a Strata-XL polymeric reverse phase cartridge. The isolated steroids were reacted with 2-hydrazino-1- methylpyridine (HMP) at 50 °C for 30 min. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used in a positive mode with multiple reaction monitoring (MRM) for the quantification of testosterone (T) and its precursor, dehydroepiandrosterone (DHEA), in saliva samples collected from twenty young Saudi professional soccer players. The analytes were separated on an ACE Ultracore 2.5 Superphenylhexyl column (150 × 3.0 mm id). The extraction recovery during the pre-treatment was >89% and gave <±20% for inter- and intra-assay precision and accuracy. The limits of quantification (LOQ) were found to be 20 pg/mL for (T and DHEA) and 50 pg/mL for Epitestosterone (EPI). The results showed no significant variation in the concentration of T between pre and post training, whereas DHEA was significantly increased after short-term exercise. These results could indicate that there is no correlation between T and its precursor DHEA level following short term physical activity. EPI concentrations could not be detected with a LOQ of 50 pg/mL in the saliva samples.
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