Preparation and evaluation of hydrophilic C18 monolithic sorbents for enhanced polar compound retention in liquid chromatography and solid phase extraction.
Hydrophilic C18 monolithic polymer sorbents were synthesized for use in solid phase extraction (SPE) and in capillary liquid chromatography (LC). The approach involved incorporating both hydrophobic and hydrophilic monomers into a monolithic material, by copolymerization of stearyl methacrylate (SMA), poly(ethylene glycol) methyl ether methacrylate (PEGMEMA) and ethylene dimethacrylate (EDMA) in the presence of selected porogens, to produce translucent mesoporous monolithic materials in bulk (SPE) or white macroporous monoliths inside fused silica capillary columns (capillary LC). A capillary column containing one of the hydrophilic C18 monoliths (i.e. poly(SMA-co-PEGMEMA-co-EDMA) with 15% (w/w) PEGMEMA) demonstrated nearly 35% reduction in retention of polycyclic aromatic compounds and greater than 40% increase in retention of phenols compared to a hydrophobic C18 monolithic column. In addition, the hydrophilic monolith demonstrated significantly improved resolution of phenols. Similar monolithic materials prepared in bulk were ground and sieved to obtain 45-65 μm particles with desired rigidity for SPE. To achieve optimum extraction performance for phenols, several parameters, including sample pH and volume, and eluent type and volume, were investigated. Under optimized experimental conditions, the method demonstrated good sensitivity (1.6 ng/mL LOD) and linearity (R(2)>0.97 for 10-200 ng/mL). Again, incorporation of 15% (w/w) PEGMEMA in the monolith increased the extraction efficiency of phenols in water from approximately 20% to 67-92% compared to a hydrophobic C18 monolithic material. Increased wettability of the sorbent by the aqueous sample matrix and the presence of hydrogen-bonding interactions are responsible for the improved retention of polar compounds.
Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, Liaoning, China.
Yun
Y
Li
Xin
X
Xie
Milton L
ML
Lee
Jiping
J
Chen
D002853:Chromatography, Liquid / Q000295:instrumentation* / Q000379:methods; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D016014:Linear Models; D008855:Microscopy, Electron, Scanning; D010316:Particle Size; D010636:Phenols / Q000302:isolation & purification*; D011084:Polycyclic Aromatic Hydrocarbons / Q000302:isolation & purification; D011109:Polymethacrylic Acids / Q000737:chemistry; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000295:instrumentation* / Q000379:methods; D014874:Water Pollutants, Chemical / Q000302:isolation & purification
D010636:Phenols; D011084:Polycyclic Aromatic Hydrocarbons; D011109:Polymethacrylic Acids; D014874:Water Pollutants, Chemical