Silva Mariana, Morante-Zarcero Sonia, Pérez-Quintanilla Damián, Marina María Luisa, Sierra Isabel
Departamento de Tecnología Química y Energética, Tecnología Química y Ambiental, Tecnología Mecánica y Química Analítica, ESCET, URJC, Móstoles, Spain.
Departamento de Química Analítica, Química Física e Ingeniería Química, Facultad de Biología, Ciencias Ambientales y Química, Universidad de Alcalá, Alcalá de Henares, Spain.
Electrophoresis. 2017 Aug;38(15):1905-1912. doi: 10.1002/elps.201600510. Epub 2017 May 8.
A method for simultaneous separation and determination of four enantiomeric pairs of β-blockers in waters by chiral CE has been developed. Off-line SPE was employed using functionalized ordered mesoporous silica as sorbent. Separation by CE was achieved using a BGE composed by methylated-β-CD (1.25% w/v) dissolved in a 50 mM phosphate buffer (pH 2.5) and 30°C, with good chiral resolution for all enantiomers. Mesoporous silica functionalized with octadecyl groups (denoted SBA15-C18) was prepared by a postsynthesis method and applied for the preconcentration of atenolol, propranolol, metoprolol, and pindolol enantiomers in waters by off-line SPE. Under optimized conditions, a preconcentration factor of 300 was achieved, employing 100 mg of SBA15-C18 as sorbent, with recoveries between 96 and 105% in tap water and good repeatability (% RSD = 7-11%, n = 6). Commercial C18 amorphous silica (ExtraBond C ) was also tested as sorbent for SPE, but results revealed better extraction capacity with higher recoveries for the SBA15-C18 material. The analytical characteristics of the off-line SPE-chiral CE method were evaluated, showing good precision, linearity, and accuracy with method quantification limits between 5.3 and 13.7 μg/L for all enantiomers. The SBA15-C18 material allowed the extraction of four enantiomeric pairs of β-blockers spiked in tap water, river water, and ground water with recoveries between 58 and 105%.
已开发出一种通过手性毛细管电泳同时分离和测定水中四对对映体β受体阻滞剂的方法。采用功能化有序介孔二氧化硅作为吸附剂进行离线固相萃取。通过毛细管电泳分离是在由溶解于50 mM磷酸盐缓冲液（pH 2.5）中的甲基化-β-环糊精（1.25% w/v）组成的背景电解质中，于30°C下实现的，所有对映体均具有良好的手性拆分效果。通过后合成方法制备了用十八烷基官能化的介孔二氧化硅（记为SBA15-C18），并将其应用于通过离线固相萃取对水中阿替洛尔、普萘洛尔、美托洛尔和吲哚洛尔对映体的预富集。在优化条件下，以100 mg SBA15-C18作为吸附剂，预富集因子达到300，自来水中的回收率在96%至105%之间，且具有良好的重复性（% RSD = 7 - 11%，n = 6）。还测试了商用C18无定形二氧化硅（ExtraBond C）作为固相萃取的吸附剂，但结果表明SBA15-C18材料具有更好的萃取能力和更高的回收率。评估了离线固相萃取-手性毛细管电泳方法的分析特性，结果表明该方法具有良好的精密度、线性和准确性，所有对映体的方法定量限在5.3至13.7 μg/L之间。SBA15-C18材料能够萃取添加到自来水、河水和地下水中的四对对映体β受体阻滞剂，回收率在58%至105%之间。
