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优化一种基于吡唑啉的荧光衍生试剂,3-萘基-1-(4-三氟甲基)-5-(4-羧基苯基)-2-吡唑啉,用于反相高效液相色谱荧光检测法对脂肪醇的灵敏柱前衍生化和痕量分析。

Tuning a pyrazoline-based fluorogenic reagent, 3-naphthyl-1-(4-trifluoromethyl)-5-(4-carboxy phenyl)-2-pyrazoline for sensitive precolumn derivatization of aliphatic alcohols and trace analysis by RP-HPLC with fluorescence detection.

机构信息

Department of Chemistry, College of Science, Sultan Qaboos University, Sultanate of Oman.

出版信息

Biomed Chromatogr. 2021 Sep;35(9):e5134. doi: 10.1002/bmc.5134. Epub 2021 May 4.

Abstract

A new member of the pyrazoline family, 3-naphthyl-1-(4-trifluoromethyl)-5-(4-carboxy phenyl)-2-pyrazoline has been evaluated as a precolumn derivatization reagent for the analysis of primary alcohols using HPLC. The simultaneous separation of eight alcohol derivatives (C -C ) within 15 min was achieved on a reverse-phase C column with an isocratic elution mode. The derivatives were detected with fluorescence at an emission wavelength of 470 nm when excited at 360 nm. The identification of the corresponding derivatives was carried out by LC-MS/MS and all showed their characteristic parent peak in negative ion mode. The proposed method was validated using normal analytical tools and was found to be excellent. As a preliminary application, our method was used to determine ethanol concentration in alcohol-containing chocolates and cough syrup.

摘要

一种新的吡唑啉类化合物,3-萘基-1-(4-三氟甲基)-5-(4-羧基苯基)-2-吡唑啉,已被评估为使用 HPLC 分析伯醇的柱前衍生试剂。在反相 C 柱上以等度洗脱模式,可在 15 分钟内同时分离八种醇衍生物(C -C )。衍生物在激发波长为 360nm 时,于 470nm 处发射荧光进行检测。通过 LC-MS/MS 对相应的衍生物进行鉴定,所有衍生物在负离子模式下均显示其特征的母峰。该方法使用常规分析工具进行了验证,结果表明该方法非常出色。作为初步应用,我们的方法用于测定含酒精巧克力和咳嗽糖浆中的乙醇浓度。

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