Brigante Tamires Amabile Valim, Miranda Luis Felippe Cabral, de Souza Israel Donizeti, Acquaro Junior Vinicius Ricardo, Queiroz Maria Eugênia Costa
School of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, 14040-903 Ribeirão Preto, Brazil.
Departamento de Química da Faculdade de Filosofia Ciências e Letras de Ribeirão Preto Universidade de São Paulo, 14040-901, Ribeirão Preto, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 1;1067:25-33. doi: 10.1016/j.jchromb.2017.09.038. Epub 2017 Sep 27.
Molecularly imprinted polymers (MIPs) were synthesized and used as sorbent for Bisphenol A (BPA) pipette tip solid-phase microextraction from urine samples and BPA analysis by gas chromatography coupled to mass spectrometry (GC-MS). The MIPs were synthesized by the sol-gel methodology. Aminopropyltriethoxysilane (APTES) and tetraethyl orthosilicate (TEOS) were used as functional monomer and cross-linking reagent, respectively. BPA and tetrabromobisphenol A (TBBPA) were evaluated as template during MIP synthesis. The BPA-based MIP displayed slightly higher extraction efficiency than the TBBPA-based dummy molecularly imprinted polymer (DMIP), but the TBBPA-based DMIP was selected as sorbent to minimize interference from leaked template. Comparison of the TBBPA-based DMIP, BPA-based MIP, and non-imprinted polymer (NIP) extraction efficiencies attested that the TBBPA-based DMIP was selective. The synthesized polymers were characterized by Scanning Electron Microscopy (SEM) and Fourier Transform Infrared spectroscopy (FTIR). The TBBPA-based DMIP was reused for over 100 times, which confirmed its robustness. The developed method was linear from 50 to 500ngmL. Precision values had coefficient of variation (CV) ranging from 4 to 14%. The accuracy relative standard deviation values (RSD) varied from -13.6 to 12.3%.
合成了分子印迹聚合物（MIPs），并将其用作从尿液样本中萃取双酚A（BPA）的移液器吸头固相微萃取吸附剂，以及用于通过气相色谱-质谱联用（GC-MS）分析BPA。MIPs采用溶胶-凝胶法合成。氨丙基三乙氧基硅烷（APTES）和正硅酸四乙酯（TEOS）分别用作功能单体和交联剂。在MIP合成过程中，评估了BPA和四溴双酚A（TBBPA）作为模板。基于BPA的MIP表现出比基于TBBPA的虚拟分子印迹聚合物（DMIP）略高的萃取效率，但选择基于TBBPA的DMIP作为吸附剂以最小化泄漏模板的干扰。对基于TBBPA的DMIP、基于BPA的MIP和非印迹聚合物（NIP）萃取效率的比较证明基于TBBPA的DMIP具有选择性。通过扫描电子显微镜（SEM）和傅里叶变换红外光谱（FTIR）对合成的聚合物进行了表征。基于TBBPA的DMIP可重复使用100多次，这证实了其耐用性。所开发的方法在50至500ng/mL范围内呈线性。精密度值的变异系数（CV）范围为4%至14%。准确度相对标准偏差值（RSD）在-13.6%至12.3%之间变化。
