摘要
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 develop an effective HPLC method based on a reaction of phenylisothiocyanate（PITC） with glucosamine（GL） in alkaline media for the determination of glucosamine hydrochloride in dosage forms.Method：Reverse phase chromatography using pre-column derivatization with phenylisothiocyanate,and ultraviolet detection（254 nm） was used to quantify the eluate.The reaction produces a phenylthiocarbamyl-glucosamine（PTC-GL） adduct which was separated on a reverse-phase（RP） column packed with Agilent TC C18（4.6 mm×250 mm,5 μm）.The mobile phase consisted of pH 5.8 phosphate buffered saline acetonitrile（90︰10） and was pumped at a flow rate of 0.8 mL·min-1,and the column temperature was maintained at 30 ℃.Galactosamine hydrochloride（Gal-HCl） was used as an internal standard.Result：The standard curves for GL-HCl showed linearity（r=0.999 1） over the selected concentration range from 350 to 550 mg·L-1 for dosage forms.The average recoveriy of glucosamine hydrochloride was 98.3%（RSD 2.3%）.Conclusion：The method was found to be specific and with excellent linearity,accuracy and precision and is well suited for the quantitation of GL-HCl in dosage forms.
出处
《中国实验方剂学杂志》
CAS
北大核心
2012年第4期116-119,共4页
Chinese Journal of Experimental Traditional Medical Formulae
