Ali Imran, Kulsum Umma, Al-Othman Zeid A, Alwarthan Abdulrahman, Saleem Kishwar
Department of Chemistry, Jamia Millia Islamia, New Delhi, India.
Department of Chemistry, College of Science, King Saud University, Riyadh, Kingdom of Saudi Arabia.
J Sep Sci. 2016 Jul;39(14):2678-88. doi: 10.1002/jssc.201600194. Epub 2016 Jul 7.
Iron nanoparticles were prepared by a green method following functionalization using 1-butyl-3-methylimidazolium bromide. 1-Butyl-3-methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid-phase membrane micro-tip extraction to separate vitamin B complex from plasma before high-performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high-performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57-39.47, 1.12-6.00 and 1.84-26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices.
采用绿色方法，在使用1-丁基-3-甲基咪唑溴化物进行功能化后制备了铁纳米颗粒。使用傅里叶变换红外光谱、能量色散X射线荧光光谱、X射线衍射、扫描电子显微镜和透射电子显微镜对1-丁基-3-甲基咪唑铁纳米颗粒进行了表征。在高效液相色谱分析之前，将这些纳米颗粒用于固相膜微尖端萃取，以从血浆中分离复合维生素B。获得的最佳条件为：吸附剂（15 mg）、振荡时间（30分钟）、pH值（9.0）、解吸溶剂[水（5 mL）+甲醇（5 mL）+氢氧化钠（0.1 N）+乙酸（d = 1.05 kg/L，pH 5.5）]、解吸体积（10 mL）和解吸时间（30分钟）。所有八种复合维生素B的回收率在60%至83%之间。使用PhE柱（250×4.6 mm，5.0μm）和水/乙腈（95:5，v/v；用0.1%甲酸调节pH值至4.0）流动相建立了一种高效液相色谱方法。流速为1.0 mL/min，检测波长为270和210 nm。容量因子、分离因子和分辨率因子的值分别为0.57 - 39.47、1.12 - 6.00和1.84 - 26.26。所建立的样品制备和色谱方法快速、选择性好、成本低、经济且可重现。所开发的方法可用于分析生物和环境基质中的这些药物。
