建立了高效阴离子交换-脉冲安培检测(HPAE-PAD)同时分离测定8种单糖和2种糖醛酸的分析方法.以CarboPac PA20阴离子交换柱为分离柱,以2 mmol/L NaOH溶液将8种单糖从分离柱上洗脱,而后用NaAc(50~200 mmol/L)梯度淋洗2种糖醛酸,淋洗液流速为0.5 mL/min,总分析时间为30 min.在优化的分离测定条件下,8种单糖和2种糖醛酸的检出限为2.5~ 14.4 μg/L(进样体积25 μL,峰面积定量).5 mg/L的10种化合物的混合标准溶液连续7次进样,峰面积的相对标准偏差为0.3%~ 1.5%.用所建立的方法测定了多糖水解液和木材半纤维素水解液中的单糖和糖醛酸含量.
A method for determination of eight monosaccharides and two uronic acids in polysaccharide and wood hemicellulose hydrolysate by high performance anion exchange chromatography with pulsed amperometric detection was established, The chromatographic separation was established on a Dionex CarboPac PA20 anion exchange column using NaOH and NaAc gradient elution (50- 200 mmol/L) at 0.5 mL/min flow rate. The total analysis time is 30 min. Detection limits of 2.5 - 14.4μg/L (25 μL injection) were achieved under the optimized conditions. RSDs of the peak area for the seven consecutive determinations of 5 mg/L eight monosaccharides and two uronic acids were 0.3% - 1.5%. The method had been applied for determination of eight monosaccharides and two uronic acids in hydrolysates of polysaccharide and wood hemicellulose.