摘要
向制备氨基葡萄糖酸的催化反应液中加入亚硝酸盐试剂,在25℃下衍生反应5 min,所得含有氨基葡萄糖盐酸盐和氨基葡萄糖酸衍生物的溶液用作高效液相色谱分析。选用AminexHPX-87H离子排斥色谱柱为固定相,以5 mmol·L^(-1)硫酸溶液为流动相进行淋洗,用示差折光检测器进行检测,提出了同时测定氨基葡萄糖盐酸盐和氨基葡萄糖酸的高效液相色谱法。2种化合物的色谱峰面积与其浓度均在50 mmol·L^(-1)以内呈线性关系,检出限(3S/N)依次为0.014,0.034 mmol·L^(-1)。方法用于5批催化反应液中氨基葡萄糖盐酸盐和氨基葡萄糖酸的测定,加标回收率依次在99.3%～100%,99.2%～102%之间;测定值的相对标准偏差均小于2.5%。
The catalytic reaction solution used for preparation of glucosaminic acid was mixed with NaNO2 as derivatizing reagent, and derivatized for 5 min at 25 ℃. The solution containing derivatives of glueosamine hydrochloride and glucosaminic acid was used for HPLC analysis, using Aminex HPX-87H ion replusive column as stationary phase and 5 mmol · L^-1 HENO4 solution as mobile phase in isocratic elution. Differential rdractive index detector was adopted in the determination. Linear relationships between values of peak area and concentration of the 2 compounds were obtained in the same range within 50 mmol ·L^-1 , with detection limits （3S/N） 0.014 mmol ·L^-1 （for glucosamine hydrochloride） and 0. 034 mmol · L^- 1 （for glucosaminic acid）. The proposed method was applied to the determination of glucosamine hydrochloride and glucosaminic acid in catalytic reaction solution, giving values of recovery in the ranges of 99.3%--100% and 99.2%--102% with RSD＇s less than 2.5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第1期69-71,74,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中央高校基本科研业务费专项资金(JUSRP11106)资助项目
