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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications
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Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications

机译：谷氨酰胺衍生的混合模型固定相的合成，用于HPLC分离结构上不同的生物活性化合物：HILIC和反相应用

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A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 mu m, 60 angstrom). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20 degrees C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10 mM) and acetonitrile with 20 degrees C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10 min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10 mM) and acetonitrile with 20 degrees C column temperature and detected at 230 or 278 nm. The best separation conditions for seven phenolic compounds was also achieved using reversed-phase HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10 mM) and acetonitrile with 20 degrees C column temperature and seven phenolic compounds could be separated and detected at 230 nm within 16 min. (C) 2014 Elsevier B.V. All rights reserved.
机译：从N-Boc-谷氨酰胺，苯胺和球形硅胶（4μm，60埃）开始合成了一种新型的混合模式固定相。制备的固定相通过IR和元素分析进行​​表征。新的固定相在苯环中带有嵌入的酰胺基，极性高的是末端酰胺基，而极性非极性的基团（苯基和烷基）。首先，这种新的混合模式固定相用于HILIC分离四个核苷酸和五个核苷。研究了pH值，流动相和温度等不同分离条件对分离过程的影响。使用HILIC等度洗脱，使用水性流动相和乙腈，柱温为20℃，可以实现核苷酸的最佳分离。在这些条件下，可以分离这四个核苷酸，并在14分钟内在265 nm处检测到。在HILIC等度洗脱下，使用含有pH = 3.25磷酸盐缓冲液（10 mM）和乙腈的水相流动相，在20°C的柱温下分离5个核苷，并在14分钟内在265 nm下检测到。计算色谱参数，如保留因子，选择性，理论塔板数和峰不对称因子，以分析流动相中的温度和水分含量对分离过程的影响。还测试了新色谱柱的核苷酸和核苷混合物，并在10分钟内分离了6种分析物。在相似条件下，将这些极性分析物在新型混合模型固定相上的色谱行为与HILIC色谱柱进行了比较。此外，将植物激素和酚类化合物分离，以观察新固定相在反相条件下的影响。使用RP-HPLC梯度洗脱，在20分钟的柱温下，使用含有pH = 2.5磷酸盐缓冲液（10 mM）和乙腈的水性流动相，分离11种植物植物激素，并在230或278 nm处检测到。还使用反相HPLC梯度洗脱，采用pH = 2.5磷酸盐缓冲液（10 mM）和乙腈的流动相，在20°C的柱温下，获得了7种酚类化合物的最佳分离条件，并且可以在7°C的温度下分离和检测7种酚类化合物16分钟内达到230 nm。 （C）2014 Elsevier B.V.保留所有权利。

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