反相高效液相色谱(RP-HPLC)系统分析维生素D3软胶囊(油性基质)  

Reverse phase high-performance liquid chromatography (RP-HPLC) system for analysis of vitamin D3 soft capsules with soybean oil matrix

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作  者:李梦瀚 丁雪梅 梁建英 LI Meng-han;DING Xue-mei;LIANG Jian-ying(Department of Pharmaceutical Analysis,School of Pharmacy,Fudan University,Shanghai 201203,China)

机构地区:[1]复旦大学药学院药物分析教研室,上海201203

出  处:《复旦学报:医学版》2019年第1期23-31,共9页Fudan University Journal of Medical Sciences

摘  要:目的开发维生素D3软胶囊(油性基质)在反相高效液相色谱(reverse phase high performance liquid chromatography,RP-HPLC)系统中的含量测定和杂质分析方法。方法RP-HPLC系统的色谱柱为AgilentZorbaxEclipseXDB-C18柱(4.6mm×250mm,5μm),检测波长265nm,柱温25℃,流速1mL/min。以乙腈混合不同比例的甲醇、水、乙醇为流动相,探究这4种流动相组分对维生素D3及其3种同分异构体在C18柱上保留行为的影响。根据保留行为研究选择合适的流动相进行含量测定和杂质分析。结果以纯乙腈为流动相时,含量测定方法回收率仅为80.55%~84.37%;而以V(乙腈)∶V(水)=90∶10为流动相时回收率显著改善(98.07%~103.23%,RSD<1.69%),同时可改善峰形,适用于含量分析。该方法呈现良好的线性[(0.52~5.2)×10^-4μmol/L,R2>0.999]和精密度(RSD<2.32%)。以V(乙腈)∶V(水)=95∶5为流动相能够排除空白油性基质峰对杂质峰的干扰,可用于杂质分析。结论本方法能在RP-HPLC系统中简单而准确地进行维生素D3软胶囊(油性基质)的含量测定和杂质分析。ObjectiveTo develop a method for the determination and impurity analysis of vitamin D3 soft capsules with soybean oil matrix in reverse phase high performance liquid chromatography (RP-HPLC) system. MethodsRP-HPLC system had Agilent Zorbax Eclipse XDB-C18 column (4.6 mm × 250 mm, 5 μm) with detection wavelength of 265 nm, column temperature of 25 ℃ and flow rate of 1 mL/min. Retention behaviors of vitamin D3 and its 3 isomers were studied by altering the mobile phase. Firstly, acetonitrile was mixed with different proportions of methanol, water and ethanol as the mobile phase to investigate the effects of these 4 mobile phase components on the retention behavior of vitamin D3 and its 3 main related substances (isomers) on a C18 column. Then, a suitable mobile phase was selected for content determination and impurity analysis according to the retention behavior study. ResultsThe recovery was only 80.55%-84.37% with 100% acetonitrile as the mobile phase.The addition of ethanol in acetonitrile was found to make remarkably significant improvement. Recovery rate was achieved between 98.07% and 103.23% with V (acetonitrile)∶ V (ethanol)=90 ∶ 10 as the mobile phase, while improving peak shape. The method showed good linearity [(0.52-5.2)× 10^-4 μmol/L, R2>0.999] and fine density (RSD<2.32%) which can be used for determination. For impurities profile,it could be achieved using V (acetonitrile)∶ V (water)=95 ∶ 5 as the mobile phase which can obviate interference from soybean oil matrix. Conclusions The method established in this experiment can easily and accurately determine the content and impurity analysis of vitamin D3 soft capsules with soybean oil matrix in a RP-HPLC system.

关 键 词:异构体 油性基质 保留行为 反相高效液相色谱(RP-HPLC) 维生素D3 软胶囊 

分 类 号:R917[医药卫生—药物分析学;医药卫生—药学]

 

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