Youjun Di, Min Zhao, Yingchun Nie, Fei Wang, Jiagen Lv
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引用次数: 18
摘要
建立了高效液相色谱(HPLC)分离-化学发光(CL)检测法对膳食补充剂中伐地那非进行灵敏分析的方法。在C18色谱柱上,以乙醇- h (3)PO(4)和乙二胺四乙酸二钠盐(Na(2)EDTA)水溶液(25.75,v/v%)为流动相,在30℃下分离伐地那非。基于伐地那非在碱性介质中与鲁米诺- k (3)Fe(CN)(6)反应的强CL增强,进行连续CL检测。在流速为0.8 mL/min时,伐地那非保留时间(t(R))为6.4 min。研究并优化了影响HPLC分辨率和CL检测的因素。伐地那非标准品在8.0 × 10(-7) ~ 1.0 × 10(-4) mol/L范围内呈线性关系。日内、日间精密度的相对标准偏差(RSD)均小于3.5%。该方法适用于口服液、葡萄酒和胶囊样品中伐地那非的含量测定。
A high-performance liquid chromatography:chemiluminescence method for potential determination of vardenafil in dietary supplement.
A flow method of high-performance liquid chromatography (HPLC) seperation and chemiluminescence (CL) detection for sensitive vardenafil analysis in dietary supplements was developed. The vardenafil separation was achieved on a C18 column at 30°C using ethanol-H(3)PO(4) and ethylenediaminetetraacetic acid disodium salt (Na(2)EDTA) aqueous solution (25 : 75, v/v%) as mobile phase. The followed continuous CL detection was conducted based on the strong CL enhancement by the presence of vardenafil to luminol-K(3)Fe(CN)(6) reaction in alkaline medium. At the flow rate of 0.8 mL/min, the vardenafil retention time (t(R)) was 6.4 min. Factors that affected the HPLC resolution and CL detection were studied and optimized. The calibration curve obtained for vardenafil standard was linear in concentration range of 8.0 × 10(-7) ~ 1.0 × 10(-4) mol/L. The relative standard deviations (RSD) of intraday and interday precision were less than 3.5%. The proposed method was applied to the vardenafil determination in oral liquid, wine, and capsule samples.