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目的:建立快捷、灵敏检测N-乙酰-D-氨基葡萄糖和D-氨基葡萄糖盐酸盐的离子色谱法。方法:采用离子色谱-积分脉冲安培检测法检测N-乙酰-D-氨基葡萄糖和D-氨基葡萄糖盐酸盐的含量,以NaOH淋洗液梯度淋洗,在CarboPac PA10高效阴离子交换柱(HPAEC)上实现分离,用Au工作电极、Ag/AgCl参比电极的脉冲安培检测器测定N-乙酰-D-氨基葡萄糖和D-氨基葡萄糖盐酸盐。结果:N-乙酰-D-氨基葡萄糖和D-氨基葡萄糖盐酸盐在0.02~20 mg/L范围内线性相关良好,相关系数r2分别为0.9999和0.9995。进样25μl、S/N=3时,方法检出限分别为0.005 mg/L和0.01 mg/L。精密性实验相对标准偏差为0.35%和0.76%;两种糖的加标回收率均在95.3%~101.6%之间。结论:建立的离子色谱-脉冲安培检测法检测N-乙酰-D-氨基葡萄糖和D-氨基葡萄糖盐酸盐,方法可靠、无需衍生、简便快捷、分离效果好、灵敏度高,可以在15 min内完成定量分析。
OBJECTIVE: To establish a rapid and sensitive method for the ion chromatography of N-acetyl-D-glucosamine and D-glucosamine hydrochloride. Methods: The contents of N-acetyl-D-glucosamine and D-glucosamine hydrochloride were detected by ion chromatography-pulse integral-amperometric detection. The samples were eluted with NaOH eluent gradient and eluted on a CarboPac PA10 high performance anion exchange column (HPAEC) , And N-acetyl-D-glucosamine and D-glucosamine hydrochloride were measured with a pulsed amperometric detector of Au working electrode and Ag / AgCl reference electrode. Results: There was a good linear correlation between N-acetyl-D-glucosamine and D-glucosamine hydrochloride in the range of 0.02-20 mg / L with correlation coefficients r2 of 0.9999 and 0.9995, respectively. Injection 25μl, S / N = 3, the detection limit of 0.005 mg / L and 0.01 mg / L. The relative standard deviations (RSDs) of the precision experiments were 0.35% and 0.76%, respectively. The spiked recoveries of the two sugars were between 95.3% and 101.6%. Conclusion: The established ion chromatography - pulse amperometric detection of N-acetyl-D-glucosamine and D-glucosamine hydrochloride, reliable, without derivative, simple and quick, good separation, high sensitivity, can be within 15 min Complete quantitative analysis.