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首页> 外文期刊>Journal of liquid chromatography and related technologies >Synthesis, purification, and stability of < beta >-diketonate europium chelate reagent, determined by RP-HPLC
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Synthesis, purification, and stability of < beta >-diketonate europium chelate reagent, determined by RP-HPLC

机译：RP-HPLC测定β-二酮酸euro螯合物的合成，纯化和稳定性

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摘要

Various estimation conditions concerned with a europium chelate labeling agent, 4-(1,1,1,2,2-pentafluoro-3,5-dioxo-pentyl)-[1,11'-biphenyl]-sulfonyl chloride (PDB-SCl), was studied, by using reversed-phase HPLC-time-resolved fluorescence detector system. Samples dissolved in acetonitrile were introduced to a TMS column; the eluent was monitored with absorbance at 280 nm, and then collected. To the fractions was added europium (Eu) solution containing tri-n-octylphosphine oxide (TOPO) and Triton X-100, and the time-resolved fluorescence intensity of the PDB-Eu chelate was measured with an off-line time-resolved fluorometer. In time-resolved fluorescence measurement, one major peak of PDB-SCl was observed, but in absorbance measurement, many peaks were observed. The fractions having time-resolved fluorescence were hydrolyzed, and the reaction solutions were analyzed by an HPLC system connected to an on-line time-resolved fluorescence detector (TRFD). There were little byproduct peaks, which were producedby reacting PDB-SCl with contaminants in the synthesized PDB-SCl powder. The stability of chlorosulfonyl group of PDB-SCl in aqueous acetonitrile solutions was also studied, and 80% of chlorosulfonyl group of PDB-SCl dissolved in 90% aqueous acetonitrile solution was hydrolyzed to sulfonic acid. However, PDB-SCl dissolved in 100% acetonitrile was stable at ambient temperature for at least 96 hours in the dark.
机译：与estimation螯合物标记剂4-（1,1,1,2,2-五氟-3,5-二氧代戊基）-[1,11'-联苯]-磺酰氯（PDB-SCl）有关的各种估算条件），使用反相HPLC-时间分辨荧光检测器系统进行了研究。将溶解在乙腈中的样品引入TMS色谱柱;用280 nm的吸光度监测洗脱液，然后收集。向馏分中加入含三正辛基氧化膦（TOPO）和Triton X-100的euro（Eu）溶液，并用离线时间分辨荧光计测量PDB-Eu螯合物的时间分辨荧光强度。 。在时间分辨荧光测量中，观察到PDB-SCl的一个主峰，但是在吸光度测量中，观察到许多峰。水解具有时间分辨荧光的级分，并通过连接在线时间分辨荧光检测器（TRFD）的HPLC系统分析反应溶液。 PDB-SCl与合成的PDB-SCl粉末中的污染物反应产生的副产物峰很少。还研究了PDB-SCl的氯磺酰基在乙腈水溶液中的稳定性，并将溶解在90％乙腈水溶液中的80％的PDB-SCl氯磺酰基水解为磺酸。但是，溶于100％乙腈的PDB-SCl在环境温度下在黑暗中稳定至少96小时。

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