Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Mahidol University, 447 Sri-Ayuddhaya Rd., Rajathevee, Bangkok 10400, Thailand.
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Mahidol University, 447 Sri-Ayuddhaya Rd., Rajathevee, Bangkok 10400, Thailand.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 15;1092:306-312. doi: 10.1016/j.jchromb.2018.06.031. Epub 2018 Jun 18.
A simple micellar electrokinetic chromatography (MEKC), using cetyltrimethyl ammonium bromide (CTAB) as micelles, for the determination of ciprofloxacin (CIP), enrofloxacin (ENR), norfloxacin (NOR) and ofloxacin (OFL) residues in surface water was developed. Peak Master was used for predicting amounts of analyte ionic forms to reduce numbers of tedious experiments in optimizing the analyte capacity factors. A baseline separation (R > 2.8) of the analytes was achieved in 7 min using 15 mM sodium dihydrogen phosphate (pH 6.0) containing 3 mM CTAB and a capillary with an effective length of 56.0 cm. A negative polarity voltage of 20 kV was used to enable the migration of the cationic micelles toward the detection site. The method shows good linearity in a range of 5 and 20 μg mL and precision (%RSD < 6.45). Percent recoveries of the method were in a range of 65.1-88.7%. The limits of detection and quantitation were in the ranges of 1-2 and 3-5 μg mL, respectively. Two steps sample clean-up and preconcentration of surface water samples by hydrophilic-lipophilic balance and fluoroquinolone-molecularly imprinted polymer were advantageous for removal of humic acids and enabling the detection of fluoroquinolone residues in the samples. Finally, the method was applied for fluoroquinolone residues analysis of surface water in Thailand.
建立了一种简单的胶束电动色谱（MEKC）方法，使用十六烷基三甲基溴化铵（CTAB）作为胶束，用于测定地表水样品中的环丙沙星（CIP）、恩诺沙星（ENR）、诺氟沙星（NOR）和氧氟沙星（OFL）残留。Peak Master 软件用于预测分析物离子形式的含量，以减少优化分析物容量因子时繁琐的实验次数。在 7 min 内，使用含有 3 mM CTAB 的 15 mM 磷酸二氢钠（pH 6.0）和有效长度为 56.0 cm 的毛细管，实现了分析物的基线分离（R > 2.8）。采用 20 kV 的负极性电压，使阳离子胶束向检测点迁移。该方法在 5 至 20 μg/mL 范围内具有良好的线性关系，精密度（%RSD < 6.45）。该方法的回收率在 65.1-88.7%之间。检测限和定量限分别为 1-2 和 3-5 μg/mL。亲水-疏水平衡和氟喹诺酮分子印迹聚合物两步法对地表水样品的净化和浓缩有利于去除腐殖酸，并能检测到样品中的氟喹诺酮残留。最后，该方法应用于泰国地表水的氟喹诺酮残留分析。
