D'Orazio Giovanni, Hernández-Borges Javier, Asensio-Ramos María, Rodríguez-Delgado Miguel Ángel, Fanali Salvatore
Instituto di Metodologie Chimiche, Consiglio Nazionale delle Ricerche (C.N.R.), Monterotondo, Roma, Italia.
Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna (ULL), La Laguna, Tenerife, España.
Electrophoresis. 2016 Jan;37(2):356-62. doi: 10.1002/elps.201500327. Epub 2015 Dec 3.
Nano-LC and CEC were coupled to MS through a nanospray or a pressurized liquid-junction interface for the simultaneous separation and determination of 11 estrogenic compounds. Different stationary phases, that is, phenyl, C18, and C18 bidentate silica hydrate, were studied. For both techniques, the phenyl stationary phase was the best option, considering separation efficiency, selectivity, and resolution. Under the optimized conditions, the baseline separation of the target compounds (including estradiol and zearalanol epimers) was achieved in less than 20 min in nano-LC-MS and less than 13 min in CEC-MS. Molecular imprinted polymer SPE was used for extracting the target compounds from mineral water samples with the analysis of nano-LC-MS. The whole molecular imprinted polymer SPE nano-LC-MS method was validated through a recovery study at two levels of concentration. Sensitivity was improved by on-column focusing technique obtaining LODs in the range 1.4-55.4 ng/L.
纳升液相色谱（Nano-LC）和毛细管电色谱（CEC）通过纳米喷雾或加压液体连接界面与质谱（MS）联用，用于同时分离和测定11种雌激素化合物。研究了不同的固定相，即苯基、C18和C18二齿硅胶水合物。对于这两种技术，考虑到分离效率、选择性和分辨率，苯基固定相是最佳选择。在优化条件下，目标化合物（包括雌二醇和玉米赤霉醇差向异构体）在纳升液相色谱-质谱联用（nano-LC-MS）中不到20分钟即可实现基线分离，在毛细管电色谱-质谱联用（CEC-MS）中不到13分钟即可实现基线分离。采用分子印迹聚合物固相萃取（SPE）从矿泉水样品中提取目标化合物，并进行纳升液相色谱-质谱联用分析。通过在两个浓度水平上的回收率研究验证了整个分子印迹聚合物固相萃取-纳升液相色谱-质谱联用方法。通过柱上聚焦技术提高了灵敏度，检测限在1.4-55.4 ng/L范围内。
