School of Pharmacy, Nanjing Medical University, Nanjing, PR China.
J Hazard Mater. 2011 Jul 15;191(1-3):177-83. doi: 10.1016/j.jhazmat.2011.04.058. Epub 2011 Apr 20.
An analytical procedure for selective extraction of sildenafil and vardenafil in herbal dietary supplements (HDSs) has been set up by using the magnetic molecularly imprinted polymers (MMIPs) as the extraction and clean-up materials, followed by high performance liquid chromatography-ultraviolet (HPLC-UV). The MMIPs were prepared by a surface molecular imprinting technique, using Fe(3)O(4) magnetite as a magnetically susceptible component, sildenafil as template molecule, 2-(trifluoromethyl) acrylic acid (TFMAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as polymeric matrix components. The MMIPs were characterized by transmission electron microscope (TEM), Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM), respectively. The heterogeneity of the MMIPs was modeled with the Freundlich isotherm equation. The resulting MMIPs had high recognition ability and fast binding kinetics for sildenafil. The MMIPs were used as dispersive solid-phase extraction (DSPE) materials to selectively extract sildenafil and vardenafil from HDSs, the contents of sildenafil and vardenafil were found to be 8.05 and 3.86 μg g(-1), respectively, and the average recoveries in spiked HDSs were 70.91-91.75% with a relative standard deviation (R.S.D.) below 7%. The MMIPs were successfully used to selectively enrich and determine sildenafil and vardenafil from HDSs.
建立了一种用于从草药膳食补充剂(HDSs)中选择性提取西地那非和伐地那非的分析方法,该方法使用磁性分子印迹聚合物(MMIPs)作为提取和净化材料,然后进行高效液相色谱-紫外(HPLC-UV)分析。MMIPs 通过表面分子印迹技术制备,以 Fe(3)O(4)磁铁矿为可磁化成分,西地那非为模板分子,2-(三氟甲基)丙烯酸(TFMAA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为聚合基质成分。分别通过透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、X 射线衍射(XRD)和振动样品磁强计(VSM)对 MMIPs 进行了表征。MMIPs 的非均质性采用 Freundlich 等温方程进行建模。所得 MMIPs 对西地那非具有高识别能力和快速结合动力学。将 MMIPs 用作分散固相萃取(DSPE)材料,从 HDSs 中选择性提取西地那非和伐地那非,发现西地那非和伐地那非的含量分别为 8.05 和 3.86 μg g(-1),在添加的 HDSs 中的平均回收率为 70.91-91.75%,相对标准偏差(R.S.D.)低于 7%。成功地使用 MMIPs 从 HDSs 中选择性地富集和测定西地那非和伐地那非。