高效阴离子交换色谱-脉冲积分安培法检测海带中的单糖、双糖和糖醛酸

Determination of Monosaccharides,Disaccharide and Uronic Acids in Laminaria japonica by High Performance Anion Exchange Chromatography with Pulsed Amperometric Detection

建立海带多糖水解液中岩藻糖、葡萄糖、氨基半乳糖、氨基葡萄糖、半乳糖、甘露糖、果糖、核糖、乳糖、半乳糖醛酸和葡萄糖醛酸11种糖类化合物的高效阴离子交换色谱-脉冲安培检测法的定性定量分析方法。采用CarboPac PA10(250 mm×4 mm)作为糖分析柱,CarboPac PA10(50 mm×4 mm)作为糖保护柱,柱温为25℃,流速为1.0 mL/min,水-NaOH-NaAc组成三元淋洗液进行多级梯度淋洗。结果表明,11种糖在各自线性范围内R^(2)不小于0.9986,方法的检出限(R_(SN)=3)在1.27~47.49 mg/kg之间,精密度相对标准偏差均小于1.78%,样品加标回收率在89.35%~115.67%之间。结果表明,该方法操作简便,线性关系良好,灵敏度和精密度高,重复性好。

A high performance anion exchange chromatography with pulsed amperometric detection method was developed for qualitatively and quantitatively analyzed 11 sugars in Laminaria japonica hydrolysate,including fucose,glucose,galactosamine,glucosamine,galactose,mannose,fructose,ribose,lactose,galacturonic acid and glucuronic acid.The separation was carried out on a CarboPac PA10 anion-exchange column(250 mm×4 mm)through gradient elution using a mobile phase consisting of water,200 mmol/L NaOH and 500 mmol/L CH3COONa at a flow rate of 1 mL/min.The column temperature was set at 25℃.The correlation coefficients(R2)of the calibration curves for all analytes were higher than 0.9986,and the detection limits(RSN=3)were in range of 1.27–47.49 mg/kg.The precision expressed as relative standard deviations(RSDs)were smaller than 1.78%and the average spiked recoveries ranged from 89.35%to 115.67%.Therefore,the developed method is simple to operate,and highly linear,sensitive,precise and reproducible.