Takegami Shigehiko, Aramoto Yuki, Konishi Atsuko
Department of Analytical Chemistry, Kyoto Pharmaceutical University, 5 Misasaginakauchi-cho, Yamashina-ku, Kyoto, 607-8414, Japan.
Anal Sci. 2022 May;38(5):813-820. doi: 10.1007/s44211-022-00100-y. Epub 2022 Mar 22.
A cyclen-based F NMR probe (F-cyclen) for hydrogen sulfide (HS) has been prepared and evaluated for its complex formation ability with Cu ions and responsivity to HS. F-Cyclen was readily synthesized by reacting cyclen with 4-(trifluoromethyl)benzyl bromide. Visible absorption spectrophotometry showed that, same as the original cyclen, F-cyclen formed a 1:1 complex with Cu ions. The F NMR signal of F-cyclen at 16.5 ppm gradually decreased in intensity with increasing CuCl concentration, with trifluoromethane sulfonic acid sodium salt (TFMSNa) used as an internal standard (0 ppm). When the Cu-F-cyclen complex was subjected to an increasing concentration of NaS (as HS donor), its corresponding F NMR signal of F-cyclen at 16.5 ppm gradually increased in intensity. The regression curve between the F NMR signal intensity ratio of F-cyclen to TFMSNa and NaS concentration showed good linearity (r = 0.986) over the NaS concentration range of 25-150 μM.
一种用于硫化氢（HS）的基于环糊精的氟核磁共振探针（F-环糊精）已被制备，并对其与铜离子的络合能力和对HS的响应性进行了评估。通过使环糊精与4-（三氟甲基）苄基溴反应，很容易合成F-环糊精。可见吸收分光光度法表明，与原始环糊精一样，F-环糊精与铜离子形成1:1络合物。以三氟甲磺酸钠盐（TFMSNa）作为内标（0 ppm），随着CuCl浓度的增加，F-环糊精在16.5 ppm处的氟核磁共振信号强度逐渐降低。当向Cu-F-环糊精络合物中加入浓度不断增加的NaS（作为HS供体）时，其在16.5 ppm处相应的F-环糊精氟核磁共振信号强度逐渐增加。在25-150μM的NaS浓度范围内，F-环糊精与TFMSNa的氟核磁共振信号强度比与NaS浓度之间的回归曲线显示出良好的线性关系（r = 0.986）。
