Anacleto Sara da Silva, de Oliveira Hanna Leijoto, da Silva Anny Talita Maria, do Nascimento Tienne Aparecida, Borges Marcella Matos Cordeiro, Silva Ricky Cássio Dos Santos, Pereira Arnaldo César, Borges Keyller Bastos
Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil.
J Chromatogr Sci. 2019 Aug 1;57(7):671-678. doi: 10.1093/chromsci/bmz036.
Herein, an organic-inorganic hybrid molecularly imprinted polymer (MIP) was successfully synthesized with albendazole sulfoxide (ABZSO) as a template and 3-(trimethoxysilyl)propyl methacrylate, a bifunctional group compound, as a single cross-linking agent. In this study, a simple method using HPLC-DAD was developed for the determination of ABZSO enantiomers in human urine using pipette tip-based molecularly imprinted polymer solid phase extraction (PT-MIP-SPE). Enantioseparation with satisfactory retention times (5.17 and 7.09 min), acceptable theoretical plates (N = 4,535 and 5,091) and strong resolution (Rs = 5.45) was performed with an Agilent® Eclipse Plus C18 (100 mm × 4.6 mm, 3.5 μm) coupled with a Chiralpak® IA column (100 mm × 4.6 mm, 3 μm), a mixture with ethanol:water (50:50, v/v) as the mobile phase, temperature at 40°C, flow rate at 0.9 mL min-1 and λ = 230 nm. Thereafter, certain parameters affecting the PT-MIP-SPE were investigated in detail and the better conditions were: 300 μL of water as washing solvent, 500 μL of ethanol:acetic acid (9:1, v/v) as eluting solvent, 20 mg of MIP, 500 μL of human urine at pH 9 and no addition of NaCl. Recoveries/relative standard deviation (RSD%) for (R)-(+)-ABZSO and (S)-(-)-ABZSO were 78.2 ± 0.2% and 69.7 ± 1.7%, respectively.
在此,以阿苯达唑亚砜(ABZSO)为模板,以双官能团化合物甲基丙烯酸3-(三甲氧基硅基)丙酯为单一交联剂,成功合成了一种有机-无机杂化分子印迹聚合物(MIP)。在本研究中,开发了一种使用高效液相色谱-二极管阵列检测法(HPLC-DAD)的简单方法,用于通过基于移液器吸头的分子印迹聚合物固相萃取(PT-MIP-SPE)测定人尿中的ABZSO对映体。使用安捷伦®Eclipse Plus C18(100 mm×4.6 mm,3.5μm)与Chiralpak®IA柱(100 mm×4.6 mm,3μm),以乙醇:水(50:50,v/v)的混合物为流动相,温度为40°C,流速为0.9 mL min-1,检测波长λ=230 nm,实现了对映体分离,保留时间令人满意(5.17和7.09分钟),理论塔板数可接受(N = 4535和5091),分离度高(Rs = 5.45)。此后,详细研究了影响PT-MIP-SPE的某些参数,最佳条件为:300μL水作为洗涤溶剂,500μL乙醇:乙酸(9:1,v/v)作为洗脱溶剂,20 mg MIP,500μL pH 9的人尿,且不添加氯化钠。(R)-(+)-ABZSO和(S)-(-)-ABZSO的回收率/相对标准偏差(RSD%)分别为78.2±0.2%和69.7±1.7%。