合成了一种以二乙烯苯和N-乙烯吡咯烷酮为单体的高分子聚合物固相萃取填料(DVB-NVP),以6种不同极性的化合物为模型化合物,结合高效液相色谱法(HPLC)对该填料进行了系统的评价,并与传统的C18填料及商品化同类型填料做对比;对填料进行了磺酸化修饰(DVB-NVP-SO3H),并将合成的填料应用于复杂基质中化合物的分析。结果表明:该填料对不同极性化合物的回收率在95.55%~101.08%之间,优于商品化C18填料,与商品化同类型填料相当。DVB-NVP对于白酒中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯的分析回收率分别为102.55%、102.99%、102.11%,相对标准偏差分别为2.11%、1.69%、0.79%;DVB-NVP-SO3H用于对猪肉中的可乐定和赛庚啶进行分析,回收率分别为89.23%和91.42%,相对标准偏差分别为8.21%和8.86%,符合生物样品分析要求。所合成的填料具有普适性,并具有较高的回收率,应用前景广泛。
A copolymer of divinylbenzene and N-vinyl pyrrolidone (DVB-NVP) was synthesized for the purpose of solid phase extraction ( SPE). Its performance as an SPE resin was evalua- ted using six model compounds having different polarities. Aqueous samples containing those compounds were applied to SPE cartridges containing the aforementioned copolymer as well as the classic C l8 and Oasis HLB for comparison, and the SPE processed samples were analyzed by using high performance liquid chromatography (HPLC) for quantitation. Then, the copolymer DVB-NVP was sulfonated to modify the surface properties. The surface modified materials were used to analyse complex samples. The results showed that DVB-NVP had high recoveries for the six compounds ranging from 95.55% to 101.08% which were better than those of the Cl 8 and were comparable to those of Oasis HLB. In applying to real samples, the recoveries for dimethyl phthalate, diethyl phthalate and dibutyl phthalate in liquor were 102.55%, 102.99% and 102. ll%, with the RSDs of 2. l 1%, I. 69%, 0.79% respectively. Simi- larly, the recoveries for clonidine and cyproheptadine in pork were 89.23% and 91.42% with the RSDs of 8.21% and 8.86%, respectively.