The Study And Application Of Microemulsion Chromatography For Environmental Organic Analysis

The actions of four phthalic acid esters and five phenols in the microemulsion chromatogram were investigated, and the conditions of separation and determination were optimized. The calibration curve equations of determining four phthalic acid esters and five phenols were fixed in the best condition, and some real samples were determined by the method. The main content of this dissertation were as follows:(1) A simple and new method for rapid screening of phthalic acid esters in plasma by microemulsion chromatogram was founded. Separations were performed on a C18 column with microemulsion as mobile phase, column temperature of 40℃, flow rate of 1.0 mL/min and measured wave length of 224 nm. The mobile phase was 4.10%(w/w) sodium dodecylsulphate, 11.14%(w/w) n-butanol, 1.0%(w/w) n-nonane, and 83.76%(w/w) aqueous disodium hydrogen phosphate-dipotassium phosphate, pH 5.5. The results demonstrate: the relative standard deviations of four analytes less than 5% and a good precision. The linear of range for the determination of phthalic acid bis-methyl ester (DMP), phthalic acid bis-buthyl ester (DBP), phthalic acid diamyl ester (DAP), phthalic acid bis-2-ethylhexyl ester (DEHP) were 0.125~25 mg/L, 0.25~30 mg/L, 0.25~30 mg/L, 0.5~25 mg/L. The detection limits(μg/L)were: 36.74 for DMP,58.31 for DBP,63.96 for DAP,87.42 for DEHP. The method was applied to determination of DMP, DBP, DAP, DEHP in sheep and human plasma. The recovery rates of each analyte were 93.5~104.8%.(2) A new method for determination of phenols in water by microemulsion chromatography was developed. Separations were performed on a C18 column with microemulsion as mobile phase, column temperature of 35℃, flow rate of 1.4 mL/min and measured wave length of 224 nm. The mobile phase was 1.0%(w/w) sodium dodecylsulphate (SDS), 4.90%(w/w) methanol, and 94.02%(w/w) aqueous acetic acid-ammonium acetate, pH 4.0. The results show that: the relative standard deviations of five phenols less than 5% and a good precision. The linear of range for the determination of hydroquinone, resorcinol, phenol, p-cresol, parachlorophenol were 0.1~10 mg/L, 0.1~16 mg/L, 0.2~12 mg/L, 0.2~20 mg/L, 0.4~20 mg/L. The detection limits (μg/L) were: 13.05 for hydroquinone, 16.38 for resorcinol, 19.71 for phenol, 23.16 for p-cresol, and 32.67 for parachlorophenol. The samples of water were disposed by solid phase extraction with GDX-502, and five phenols in the river water were determinated by the founded method. The recovery rates of each phenol were 93.3~103.0%, except for hydroquinone and resorcinol.