Funazo K, Tanaka M, Yasaka Y, Takigawa H, Shono T
Department of Chemistry, Osaka Prefectural College of Technology, Japan.
J Chromatogr. 1989 Nov 3;481:211-9. doi: 10.1016/s0021-9673(01)96765-2.
New UV-labelling agents have been synthesized, which are designed to convert monocarboxylic acids into their highly UV-absorbing derivatives for enhancement of the sensitivities of UV detection in high-performance liquid chromatography. The reagents are p-nitrobenzyl, 3,5-dinitrobenzyl and 2-(phthalimino)ethyl p-toluenesulphonates. Each has been prepared by reaction of p-toluenesulphonyl chloride with p-nitrobenzyl alcohol, 3,5-dinitrobenzyl alcohol or N-(hydroxyethyl)phtalimide, respectively, in the presence of sodium hydroxide, and they are stable in the solid state for at least 6 months. Monocarboxylic acids were derivatized to their p-nitrobenzyl, 3,5-dinitrobenzyl or 2-(phthalimino)ethyl esters with each of the above reagents, respectively, then determined by high-performance liquid chromatography with UV detection. In the UV-labelling with each reagent, 18-crown-6 was used as the catalyst. The effects of the reaction solvent, reaction temperature and time and the concentrations of each reagent and the catalyst were also examined.
已合成了新型紫外标记试剂，其设计目的是将一元羧酸转化为具有高紫外吸收性的衍生物，以提高高效液相色谱中紫外检测的灵敏度。这些试剂是对硝基苄基、3,5 - 二硝基苄基和对甲苯磺酸2 -（邻苯二甲酰亚氨基）乙酯。它们分别是通过对甲苯磺酰氯与对硝基苄醇、3,5 - 二硝基苄醇或N -（羟乙基）邻苯二甲酰亚胺在氢氧化钠存在下反应制备的，并且在固态下至少稳定6个月。分别用上述每种试剂将一元羧酸衍生化为其对硝基苄基、3,5 - 二硝基苄基或2 -（邻苯二甲酰亚氨基）乙酯，然后通过带紫外检测的高效液相色谱法进行测定。在使用每种试剂进行紫外标记时，使用18 - 冠 - 6作为催化剂。还研究了反应溶剂、反应温度和时间以及每种试剂和催化剂浓度的影响。
