Departamento de Medio Ambiente, INIA, Ctra de La Coruña Km 7, 28040 Madrid, Spain.
Talanta. 2010 Mar 15;80(5):1782-8. doi: 10.1016/j.talanta.2009.10.023. Epub 2009 Dec 11.
An analytical methodology incorporating a molecularly imprinted solid-phase extraction procedure (MISPE) has been developed for the determination of parabens in environmental solid samples. Four different polymers were prepared combining the use of acetonitrile or toluene as porogen, and 4-vinylpyridine (VP) or methacrylic acid (MAA) as monomer, using benzylparaben (BzP) as a template molecule. Although all the polymers were able to recognize the template in rebinding experiments, the MIP prepared in toluene using MAA showed better performance. This polymer was also capable of recognizing other parabens (methyl, ethyl, isopropyl, propyl, isobutyl, butyl and benzylparaben) allowing to develop an appropriated MISPE procedure for this family of compounds. The extraction of the parabens from environmental solid samples was performed by ultrasonic assisted extraction in small columns (SAESC), and this procedure next to MISPE as clean-up step followed by HPLC-UV determination was successfully used for the determination of parabens in soil and sediment samples of different locations. Recoveries ranging from 80% to 90% have been achieved depending on the compound and the samples, and limits of detection (LODs) were under 1 ng g(-1) for all the compounds, making this method suitable for the determination of parabens in environmental solid matrices. The method was further applied to the determination of paraben contents in real samples, founding levels up to 11.5 ng g(-1) in sea sediments.
已开发出一种分析方法,其中包含分子印迹固相萃取程序(MISPE),用于测定环境固体样品中的对羟基苯甲酸酯。使用乙腈或甲苯作为致孔剂,使用 4-乙烯基吡啶(VP)或甲基丙烯酸(MAA)作为单体,结合使用苯佐卡因(BzP)作为模板分子,制备了四种不同的聚合物。尽管所有聚合物在重结合实验中均能够识别模板,但在甲苯中使用 MAA 制备的 MIP 表现出更好的性能。该聚合物还能够识别其他对羟基苯甲酸酯(甲基、乙基、异丙基、丙基、异丁基、丁基和苯佐卡因),从而可以为该化合物家族开发适当的 MISPE 程序。通过在小柱中进行超声辅助提取(SAESC),从环境固体样品中提取对羟基苯甲酸酯,然后通过 HPLC-UV 测定进行 MISPE 作为净化步骤,成功地用于测定不同地点的土壤和沉积物样品中的对羟基苯甲酸酯。根据化合物和样品的不同,回收率范围为 80%至 90%,所有化合物的检测限(LOD)均低于 1 ng g(-1),这使得该方法适用于测定环境固体基质中的对羟基苯甲酸酯。该方法进一步应用于实际样品中对羟基苯甲酸酯含量的测定,在海沉积物中发现的含量高达 11.5 ng g(-1)。