羟基和甲氧基取代苯甲醛在亚硫酸氢钠-乙酸乙酯-水两相中分配系数的测定  

Partition Coefficients of Hydroxyl and Methoxy Substituted Benzaldehyde Compounds in Sodium Bisulfite-Ethyl Acetate-Water Two-Phase Solvent System

作　　者：王金[1] 巢志茂[1] 王秀娟[2] 郗砚彬[1] 龚慕辛[2] 王地[2] 

机构地区：[1]中国中医科学院中药研究所,北京100700 [2]首都医科大学中医药学院,北京100069

出　　处：《中国药学杂志》2011年第13期1034-1037,共4页Chinese Pharmaceutical Journal

基　　金：人事部留学人员科技活动择优资助项目(国人厅发[2006]164号)

摘　　要：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 4 hydroxyl and methoxy substituted benzaldehyde compounds in sodium bisulfite-ethyl acetate-water two-phase solvent system,and study the possibility of extracting natural aldehyde compounds by means of sodium bisulfite addition reaction and hydrochloric acid acidulation.METHODS Liposoluble aldehyde compounds were transformed into water soluble sodium α-hydroxyalkane sulfonate derivatives by a sodium bisulfite addition reaction,then transferred into the aqueous phase in hydrophobic two-phase solvent system.The partition coefficients of 4 hydroxyl and methoxy substituted benzaldehyde compounds were measured by high performance liquid chromatography in sodium bisulfite-ethyl acetate-water two-phase solvent system of different ratios.The original aldehyde compounds were recovered from sodium α-hydroxyalkane sulfonate derivatives by adding hydrochloric acid and the second extraction.RESULTS The partition coefficients of aldehyde compounds decreased quickly along with the increasing ratios of sodium bisulfite in sodium bisulfite-ethyl acetate-water two-phase solvent system,and then reached a balance.CONCLUSION Liposoluble aldehyde compounds can be transformed into water soluble sodium α-hydroxyalkane sulfonate derivatives by sodium bisulfite addition reaction and then recovered by hydrochloric acid acidulation.Some natural aldehyde compounds can be specificly extracted and isolated by sodium bisulfite addition reaction followed by acidulation and twice partition extractions.

关 键 词：醛 苯甲醛 亚硫酸氢钠 分配系数 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]