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高效液相色谱法测定伏格列波糖片有关物质
高效液相色谱法测定伏格列波糖片有关物质
祝传勇,刘 宁,李 强,王迷娟

北京协和药厂,北京 102600
Determination of related substances in voglibose tablets by HPLC
(Beijing Union Pharmaceutical Factory, Beijing 102600,China)

摘要参考文献相关文章

起始页:443

摘要:目的:用高效液相色谱法(high performance liquid chromatography,HPLC)检测伏格列波糖片有关物质。方法:用Shodex柱Asahipak NH2-50 4E(250 mm×4.6 mm,5 μm)做色谱柱,以磷酸盐缓冲液作为流动相A,以乙腈做为流动相B,进行梯度洗脱;荧光检测器,激发波长350 nm,发射波长430 nm,柱后衍生;调节流动相流速,使伏格列波糖峰保留时间约为20 min;荧光试剂溶液的流速与流动相的流速相同,反应浴温度为100 ℃,冷却浴温度约为15 ℃。结果:用本法检测伏格列波糖片有关物质时,伏格列波糖与辅料及杂质A、杂质B、杂质C的分离度均大于1.5,杂质A、杂质B、杂质C的回收率均大于90%,RSD均小于1.5%,当色谱条件发生微小改变时,对有关物质的检测无影响。结论:本法能有效检测出伏格列波糖片的有关物质,专属性高、分离度好、结果准确可靠。

关键词:伏格列波糖片;有关物质;高效液相色谱法

通讯作者:

基金项目:

作者简介:祝传勇,男,研究实习员,主要从事药物分析研究。

Abstract:Objective: To develop an high performance liquid chromatography (HPLC) method for determining related substances in voglibose tablets.Methods: Phosphate buffer was used as mobile phase A, acetonitrile as mobile phase B, and gradient elution was carried out on a Shodex Asahipak NH2-50 4E (250 mm×4.6 mm, 5 μm) column. To regulate the flow of Voglibose retention time is about 20 minutes,and the flow rate of the fluorescent reagentis the same as that of the mobile phase. After derivation with fluorescence reagent at 100 ℃ and then cooled at 15 ℃, the effluents were detected with fluoescence detector with excitation wavelength at 350 nm and emission wave length at 430 nm.Results: This method was applied to detect the related substances in voglibose tablets,the results showed that voglibose was well separated from other impurities (R>1.5). All the recoveries of impurity A, impurity B and impurity C were higher than 90% (RSD<1.5%).Conclusion: This method has satisfactory repeatability, sensitivity and specificity.

Key words:voglibose tablets; related substance; HPLC

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