[18O]血栓烷B3作为内标物的气相色谱-选择离子监测微量测定

Takanori Hishinuma , Yukiko Nakagawa , Tohru Yamazaki , Seiji Hiraku , Michinao Mizugaki
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引用次数: 3

摘要

我们设计了一种简单有效的纯化方法,用于TXA3水解产物血栓素B3 (TXB3)的微量测定。[18O2]通过重复碱催化甲酯衍生物在[18O]水中水解合成TXB3,获得TXB3气相色谱/选择离子监测(GC/SIM)的内标(IS)。制备了甲酯(ME)-甲氧基肟(MO)-二甲基异丙基硅基(DMIPS)醚衍生物,采用GC/SIM法测定TXB3在m/z 668和IS在m/z 672的离子。在10 pg ~ 10 ng的范围内具有良好的线性响应。用二十碳五烯酸(EPA)或二十二碳六烯酸(DHA)培养的人红细胞白血病(HEL)细胞培养液检测了TXB3的水平。该方法可用于生物样品中3系血栓素的测定。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Microdetermination of the Thromboxane B3 Gas Chromatography-Selected-Ion Monitoring Using [18O]Thromboxane B3 as an Internal Standard

We devised a simple and effective purification for the microdetermination of thromboxane B3 (TXB3), a hydrolysis product of TXA3. [18O2]TXB3 was synthesized by the repeated base-catalyzed hydrolysis of methyl ester derivatives in [18O]water, to obtain an internal standard (IS) for the gas chromatography/selected ion monitoring (GC/SIM) of TXB3. The methyl ester (ME)-methoxime (MO)-dimethylisopropylsilyl (DMIPS) ether derivative was prepared, then GC/SIM was carried out by monitoring the ion at m/z 668 for TXB3 and that at m/z 672 for IS. A good linear response over the range of 10 pg ∼ 10 ng was demonstrated. We were able to detect the levels of TXB3 in the medium of human erythroleukemia (HEL) cell cultured with eicosapentaenoic acid (EPA) or docosahexaenoic acid (DHA). This method can be used to determine 3-series thromboxane in biological samples.

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