College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, 510006, China.
Anal Bioanal Chem. 2014 Feb;406(5):1551-6. doi: 10.1007/s00216-013-7541-6. Epub 2013 Dec 18.
A method was developed to sensitively determine safranine T in wolfberry by molecularly imprinted solid-phase extraction (MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC-LIF). The MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using safranine T, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions and the morphologies of inner polymers were characterized by scanning electron microscopy (SEM). The mean recoveries of safranine T in wolfberry ranged from 91.2 % to 92.9 % and the intraday and interday relative standard deviation (RSD) values all ranged from 3.4 % to 4.2 %. Good linearity was obtained over 0.001-1.0 μg mL(-1) (r = 0.9999) with a detection limit (S/N = 3) of 0.4 ng g(-1). Under the selected conditions, enrichment factors of over 90-fold were obtained and the extraction on the monolithic column effectively cleaned up the wolfberry matrix. The results demonstrated that the proposed MISPE-HPLC-LIF method could be applied to sensitively determine safranine T in wolfberry.
建立了一种通过分子印迹固相萃取（MISPE）与高效液相色谱和激光诱导荧光检测（HPLC-LIF）联用灵敏测定枸杞中藏花红 T 的方法。采用水相原位聚合法制备 MISPE 毛细管整体柱，以藏花红 T、甲基丙烯酸（MAA）和乙二醇二甲基丙烯酸酯（EDMA）分别为模板、功能单体和交联剂。在优化条件下考察了自制 MISPE 毛细管整体柱的性能，包括容量和特异性，并通过扫描电子显微镜（SEM）对聚合物的形貌进行了表征。在枸杞中，藏花红 T 的平均回收率在 91.2%至 92.9%之间，日内和日间相对标准偏差（RSD）值均在 3.4%至 4.2%之间。在 0.001-1.0 μg mL(-1)（r = 0.9999）范围内具有良好的线性关系，检测限（S/N = 3）为 0.4 ng g(-1)。在选定的条件下，可获得超过 90 倍的富集因子，并且整体柱上的萃取有效地净化了枸杞基质。结果表明，所提出的 MISPE-HPLC-LIF 方法可用于灵敏测定枸杞中藏花红 T。
