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Cyclic imines (CIs) produced by microalgal species that accumulate in the food chains of marine organisms are novel biotoxins that do not belong to the classic group of marine biotoxins. In the past, CIs were found only in limited areas; however, in recent years, rapid changes in marine ecosystems have led to widespread CIs and increased exposure to toxic risks. In this study, we analyzed seven CI toxins, GYM-A, SPX (13-desmethyl spirolide C, 13, 19-dideMe spirolide C, 20-methyl spirolide G), and PnTX-E, F, and G, using LC/MRM-MS. Shellfish samples were purchased from a domestic Korean fish market (67 samples in 2021 and 216 samples in 2022). The entire body of the shellfish was ground and extracted with 50% methanol, followed by lipophilic-specific SPE. Only GYM-A, PnTX-G, and 13-desmethyl spirolide C were detected in all analyzed samples. The maximum concentrations of GYM-A is maximum 179 ppt (ng/kg) in Crassostrea nippona (March 2022), PnTX-G is maximum 7 ppt in Anadara broughtonii (April 2022), 13-desmethyl SPX C is maximum 58 ppt in Crassostrea nippona (April 2022). The southern coast exhibited the highest frequency of detection of these toxins, which was attributed to elevated sea-surface temperatures, aligned with conducive conditions for toxin-producing phytoplankton. According to the monitoring results, there were no significant CI toxins in the shellfish; however, it is important to monitor CI toxin accumulation in shellfish because of their high risk of toxicity.
Cyclic imines (CIs) produced by microalgal species that accumulate in the food chains of marine organisms are novel biotoxins that do not belong to the classic group of marine biotoxins. In the past, CIs were found only in limited areas; however, in recent years, rapid changes in marine ecosystems have led to widespread CIs and increased exposure to toxic risks. In this study, we analyzed seven CI toxins, GYM-A, SPX (13-desmethyl spirolide C, 13, 19-dideMe spirolide C, 20-methyl spirolide G), and PnTX-E, F, and G, using LC/MRM-MS. Shellfish samples were purchased from a domestic Korean fish market (67 samples in 2021 and 216 samples in 2022). The entire body of the shellfish was ground and extracted with 50% methanol, followed by lipophilic-specific SPE. Only GYM-A, PnTX-G, and 13-desmethyl spirolide C were detected in all analyzed samples. The maximum concentrations of GYM-A is maximum 179 ppt (ng/kg) in Crassostrea nippona (March 2022), PnTX-G is maximum 7 ppt in Anadara broughtonii (April 2022), 13-desmethyl SPX C is maximum 58 ppt in Crassostrea nippona (April 2022). The southern coast exhibited the highest frequency of detection of these toxins, which was attributed to elevated sea-surface temperatures, aligned with conducive conditions for toxin-producing phytoplankton. According to the monitoring results, there were no significant CI toxins in the shellfish; however, it is important to monitor CI toxin accumulation in shellfish because of their high risk of toxicity.
Due to the increase in the rate of male and female infertility, assisted fertilization practices are currently adopted as valid support for couples unable to get pregnant. Analytical approaches for fertility hormone dosages are constantly being developed, following the technological progress of fertilization methods that have evolved for more than a century. Indeed, the analysis of fertility hormones in serum samples is a common clinical practice to check the fertility state, but absolute quantification of these hormones is a great challenge due to biological variability and low serum concentrations. Currently, ELISA (enzyme-linked immunosorbent assay) based methods are the most used analytical techniques to quantify hormones in blood in clinical settings. The current Article discusses the development of a liquid chromatography-tandem mass spectrometry method (LC-MS/MS) to monitor multiple fertility hormones of a protein nature in a single chromatographic run, i.e., LH (luteinizing hormone), FSH (follicle-stimulating hormone), TSH (thyroid-stimulating hormone), AMH (anti-Mullerian hormone), adiponectin, ghrelin, leptin, glucagon, and obestatin. Particular attention has been paid to the AMH hormone, whose ELISA-based quantification is known to be controversial due to the poor reproducibility between the various kits used. For AMH, the internal standard method was used for the quantitative determination to compare mass spectrometry data to the ELISA assays performed by an accredited analysis laboratory on a cohort of samples from women aged between 18 and 60 years. The ability to monitor multiple transitions by LC-MRM/MS ensured both high specificity and high selectivity, which is necessary for the quantification of protein and steroid hormones, besides improvements in data reproducibility and reduced analysis times and costs.
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