含磷试剂衍生-核磁共振技术分析醇类化合物

Analysis of Alcohols with Phosphorylation-Nuclear Magnetic Resonance

本研究以含磷试剂二苯基次膦酰氯、三氯氧磷、2-氯-4,4,5,5-四甲基-1,3,2-二噁磷杂戊环(CTMP)为衍生试剂,对5种醇类化合物奎宁醇、硫二甘醇、甲基二乙醇胺、三乙醇胺、二异丙胺基乙醇进行衍生化,然后进行^(31)P{~1H}-NMR谱测定。实验考察了衍生试剂、衍生溶剂、缚酸剂作用,以及衍生时间和温度对衍生效率的影响。结果表明,以二苯基次膦酰氯为衍生试剂,二甲基甲酰胺(DMF)为衍生溶剂,吡啶作为缚酸剂,50℃衍生1h衍生条件下,5种目标化合物奎宁醇、硫二甘醇、甲基二乙醇胺、三乙醇胺、二异丙胺基乙醇的检出限(S/N=3)依次为8.90、7.33、5.95、5.96、10.16μg/mL。该方法具有良好的专一性和稳定性。同时考察了水样基质中该衍生方法的回收率。

In this work,we use phosphorus reagent diphenylphosphinyl chloride,screened as derivative reagent,to label five alcohols including,quinuclidinol,thiodiglycol,N-methyl diethanolamine,triethanolamine,N,N-diisopropyl aminoethaneol in DMF at 50℃for 1 h under pyridine catalysis.The derivative products were determined by alP{1H}-NMR and showed good stability.The detection limit(S/N=3)of these alcohols were 8.90/,g/mL,7.33μg/mL,5.95/xg/mL,5.96μg/mL,10.16μg/mL respectively,for quinuclidinol,thiodiglycol,N-methyl diethanolamine,triethanolamine,N,N-diisopropyl aminoethane.