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目的:采用异硫氰酸苯酯柱前衍生化高效液相色谱法测定复方制剂中盐酸氨基葡萄糖的含量。方法:以氨基半乳糖为内标,异硫氰酸苯酯为柱前衍生剂,采用Agilent TC C18(4.6 mm×250 mm,5μm)色谱柱,流动相10 mmol.L-1pH 5.8的磷酸盐缓冲液-乙腈(90!10),检测波长254 nm,流速0.8 mL.min-1,柱温30℃。结果:盐酸氨基葡萄糖质量浓度在350～550 mg.L-1,经衍生化后其衍生物峰面积与内标衍生物峰面积的比值与盐酸氨基葡萄糖浓度呈线性相关(r=0.999 1)。制剂中盐酸氨基葡萄糖含量测定的平均回收率98.3%(RSD 2.3%)。结论:异硫氰酸苯酯柱前衍生化高效液相色谱法测定结果准确灵敏、方法可靠,适用于复方制剂中等复杂样品中盐酸氨基葡萄糖的含量测定。
OBJECTIVE: To determine the content of glucosamine hydrochloride in compound preparations by high performance liquid chromatography (HPLC) with phenylisothiocyanate pre column. Methods: Amino-galactose was used as internal standard. Phenylisothiocyanate was used as a pre-column derivatization reagent. The mobile phase consisted of 10 mmol.L-1 pH 5.8 phosphate with Agilent TC C18 (4.6 mm × 250 mm, 5 μm) Buffer-acetonitrile (90 10), detection wavelength 254 nm, flow rate 0.8 mL.min-1, column temperature 30 ℃. Results: The concentration of glucosamine hydrochloride in the range of 350-550 mg · L-1 showed a linear correlation (r = 0.999 1) with the ratio of the peak area of the derivative to the peak area of the internal standard derivative after derivatization. The average recovery of glucosamine hydrochloride in the formulation was 98.3% (RSD 2.3%). Conclusion: The results of pre-column derivatization with phenylisothiocyanate are accurate and sensitive, and the method is reliable. The method is suitable for the determination of glucosamine hydrochloride in medium-complex samples of compound preparation.