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目的采用Waters 2695型高效液相色谱仪建立定量分析氨基葡萄糖拟肽的方法。方法以HypersilODS2(4.6mm×250mm,5μm)为分离柱,流动相为5 mmoL/L pH=7.5的磷酸二氢钾-乙腈体系(70∶30,体积分数),检测波长为200nm,流速为1.0mL/min。结果 4种物质的浓度分别在25~800μg/mL(r=0.999 9,TAG-Phe),40~1 000μg/mL(r=0.999 3,TAG-Leu),27~600μg/mL(r=0.999 1,TAG-Glu)及50~600μg/mL(r=0.999 1,TAG-Val)时呈良好的线性关系,对应的定量限(S/N=10)分别为:20.00,35.54,25.00和49.00μg/mL。检测限(S/N=3)依次为:4.50,15.30,13.45和19.30μg/mL。平均回收率在98.75%~101.56%之间,日内及日间精密度均小于1.37%。结论该方法简便,快速,专属性强,适用于氨基葡萄糖拟肽类物质的含量测定。
Objective To establish a method for the quantitative analysis of glucosamine peptidomimetic using Waters 2695 high performance liquid chromatography. Methods Hypersil ODS2 (4.6mm × 250mm, 5μm) was used as the separation column. The mobile phase consisted of 5 mmoL / L potassium dihydrogen phosphate-acetonitrile system pH = 7.5 with a detection wavelength of 200 nm and a flow rate of 1.0 mL / min. Results The concentrations of four substances were 25 ~ 800μg / mL (r = 0.999 9, TAG-Phe), 40 ~ 1 000μg / mL (r = 0.999 3, TAG-Leu) and 27 ~ 600μg / mL 1, TAG-Glu) and 50-600μg / mL (r = 0.999 1, TAG-Val). The corresponding limits of quantitation (S / N = 10) were 20.00, 35.54, 25.00 and 49.00 μg / mL. The limits of detection (S / N = 3) were: 4.50, 15.30, 13.45 and 19.30 μg / mL. The average recoveries ranged from 98.75% to 101.56% with intra-day and intra-day precision less than 1.37%. Conclusion The method is simple, rapid, specific and suitable for the determination of glucagon peptidomimetics.