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Characterization of ovatoxin-h, a new ovatoxin analog, and evaluation of chromatographic columns for ovatoxin analysis and purification

机译:Ovatoxin-H,一种新型卵毒素模拟的表征和卵巢谱分析和纯化的色谱柱评价

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摘要

The presence of Ostreopsis cf. ovata on the Mediterranean coast represents a serious concern to human health due to production of toxins–putative palytoxin and ovatoxins (ovatoxin-a, -b, -c, -d, -e, -f and -g). However, purified ovatoxins are not widely available and their toxicities are still unknown. In the present study, we report on HR LC-MS/MS analysis of a French Ostreopsis cf. ovata strain (IFR-OST-0.3 V) collected at Villefranche-sur-Mer (France) during a bloom in 2011. Investigation of this strain of Ostreopsis cf. ovata cultivated in our laboratory by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS) confirmed the production of ovatoxins -a to–e and revealed the presence of a new ovatoxin analogue, named ovatoxin-h. Ostreopsis cf. ovata extracts were pre-purified by Sephadex LH-20 to obtain a concentrated fraction of ovatoxins (OVTXs). This method provided a recovery of about 85% of OVTXs and a cleanup efficiency of 93%. Different stationary phases were tested with this fraction of interest to elucidate the structure of the new OVTX congener and to obtain purified ovatoxins. Eight reversed phase sorbents were evaluated for their capacity to separate and purify ovatoxins. Among them Kinetex C18, Kinetex PFP and Uptisphere C18-TF allowed for best separations almost achieving baseline resolution. Kinetex C18 is able to sufficiently separate these toxins, allowing us to identify the toxins present in the extract purified by Sephadex LH-20, and to partly elucidate the structure of the new ovatoxin congener. This toxin possesses one oxygen atom less and two hydrogens more than ovatoxin-a. Investigations using liquid chromatography coupled to high resolution tandem mass spectrometry suggest that the part of the molecule where ovatoxin-h differs from ovatoxin-a is situated between C42 and C49. Uptisphere C18-TF was proposed as a first step preparative chromatography as it is able to separate a higher number of ovatoxins (especially ovatoxin-d and ovatoxin-e) and because it separates ovatoxins from unknown compounds, identified using full scan single quadrupole mass spectrometry. After pre-purification with Sephadex LH-20, purification and separation of individual ovatoxins was attempted using an Uptisphere C18-TF column. During recovery of purified toxins, problems of stability of OVTXs were observed, leading us to investigate experimental conditions responsible for this degradation.
机译:存在鸵鸟的CF.由于毒素推定的腭毒素和卵酸(Ovatoxin-A,-C,-C,-D,-E,-F和-G),地中海海岸上的卵塔代表了人类健康的严重关切。然而,纯化的Ovatoxins并不广泛可用,并且它们的毒性仍然未知。在本研究中,我们报告了法国鸵鸟的HR LC-MS / MS分析。 2011年在盛开的盛开期间在Villefranche-Sur-Mer(法国)收集的卵巢菌株(IFR-OST-0.3V)。调查这种鸵鸟菌株的伤害。通过超高效液相色谱法培养的卵巢通过超高效液相色谱法耦合到高分辨率质谱(UHPLC-HRMS)证实了Ovatoxins-A至-e的产生并揭示了新的卵巢蛋白类似物的存在,称为Ovatoxin-h。鸵鸟CF.通过Sephadex LH-20预先纯化卵巢提取物,得到浓缩的卵子毒素(OVTX)。该方法提供了约85%的OVTX的回收率和93%的清洁效率。用这种感兴趣的群体测试不同的固定相,以阐明新的OVTX Congener的结构并获得纯化的Ovatoxins。评估八个反相吸附剂的能力分离和纯化过毒素。其中Kinetex C18,Kinetex PFP和Uptisphere C18-TF允许最好的分离,几乎实现基线分辨率。 Kinetex C18能够足够地分离这些毒素,使我们鉴定由Sephadex LH-20纯化的提取物中存在的毒素,并部分地阐明新的Ovatoxin Congener的结构。该毒素具有比Ovatoxin-A更少的氧原子少和两个氢。使用液相色谱耦合到高分辨率串联质谱的研究表明,Ovatoxin-H与Ovatoxin-A不同的分子部分位于C42和C49之间。提出了上行苯甲基-TF作为第一步制备色谱,因为它能够分离更多数量的卵酸(特别是Ovatoxin-D和Ovatoxin-e),并且因为它将Ovatoxins与未知化合物分离,使用全扫描单Quadruprole质谱法鉴定。用Sephadex LH-20预纯化后,使用同比单苯甲酸C18-TF柱试图纯化和单个Ovatoxins的分离。在纯化毒素的回收过程中,观察到OVTX的稳定性问题,导致我们研究负责这种降解的实验条件。

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