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目的以羟基和甲氧基取代的4个苯甲醛系列化合物为对象,测定它们在亚硫酸氢钠-乙酸乙酯-水两相体系中的分配系数,采用亚硫酸氢钠加成和盐酸酸化的方法研究提取和分离天然醛类化合物的可行性。方法采用亚硫酸氢钠加成反应,将脂溶性的醛类化合物转化成水溶性的α-羟基磺酸钠衍生物,使醛类化合物从有机相转移到水相。采用高效液相色谱法测定不同比例的亚硫酸氢钠-乙酸乙酯-水两相体系中这些化合物在上相与下相之间的分配系数。采用盐酸酸化和分配萃取,实现α-羟基磺酸钠衍生物还原为原有的醛类化合物。结果醛类化合物的分配系数,随着亚硫酸氢钠-乙酸乙酯-水两相体系中亚硫酸氢钠比例的增加急剧减小,并达到平衡。结论通过亚硫酸氢钠加成反应和盐酸酸化,使脂溶性的醛类化合物经水溶性的α-羟基磺酸钠衍生物还原到原始的醛类化合物,经两次萃取,可以实现天然产物中醛类化合物专属性的提取和分离。
OBJECTIVE To determine the partition coefficients of four benzaldehydes substituted with hydroxyl and methoxy groups in sodium bisulfite-ethyl acetate-water two-phase system, and the sodium bisulfite addition and hydrochloric acid acidification Methods to study the feasibility of extracting and separating natural aldehydes. Methods Adopting sodium bisulfite addition reaction, the fat-soluble aldehydes were transformed into water-soluble sodium α-hydroxy sulfonate derivatives to transfer the aldehydes from the organic phase to the aqueous phase. The partition coefficients of these compounds between the upper and lower phases in different ratios of sodium bisulfite-ethyl acetate-water two-phase system were determined by high performance liquid chromatography. Hydrochloric acid acidification and distribution extraction, the α-hydroxy-sodium sulfonate derivatives to achieve the original aldehyde compounds. Results The partition coefficient of aldehydes decreased sharply with the increase of the proportion of sodium bisulfite in the sodium bisulfite-ethyl acetate-water two-phase system and reached equilibrium. Conclusion Sodium bisulfite addition reaction and hydrochloric acid acidification make the fat-soluble aldehyde compound reduced to the original aldehyde compound through the water-soluble sodium α-hydroxy sulfonate derivative. After twice extraction, Extraction and isolation of aldehydes.