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建立了基于双层固相萃取-超高液相色谱(SPE-UPLC)法测定水中苯环类有机酸的检测方法。研究结果表明,80 mg质量比为1∶1的Lichrolut EN/ENVi-18双层填料在1.3 m L/min流量条件下,实现了混合苯环类有机酸的高效富集浓缩,1 m L甲醇洗脱9种苯环类有机酸的萃取率为100%±20%。测定条件如下,以20 mmol/L磷酸盐缓冲溶液(正磷酸调节p H值为2.10)∶纯水∶乙腈=5∶75∶20为流动相,以0.2 m L/min流速进行淋洗,色谱柱为ACQUITY UPLC BEH C18,柱温为25℃,TUV检测器,检测波长为210 nm,进样量为10μL。本方法可以同时测定水中9种苯环类有机酸,在给定浓度范围内各有机酸的峰面积与浓度具有良好的线性关系。平均回收率为79%~102.8%,RSD为0.26%~5.1%(n=6)。将该方法用于东太湖某水厂各工段水样检测,结果令人满意。
A method for the determination of benzene ring organic acids in water by double-layer solid-phase extraction coupled with ultra-high performance liquid chromatography (SPE-UPLC) was established. The results showed that 80 mg Lichrolut EN / ENVi-18 double-layer packing with a mass ratio of 1: 1 achieved high concentration and concentration of mixed benzene ring organic acids under the flow rate of 1.3 m L / min. Elution of 9 kinds of benzene ring organic acid extraction rate of 100% ± 20%. The measurement conditions were as follows: a 20 mmol / L phosphate buffer solution (pH = 2.10 with orthophosphoric acid): pure water: acetonitrile = 5:75:20 as a mobile phase and eluted at a flow rate of 0.2 mL / The column was an ACQUITY UPLC BEH C18 with a column temperature of 25 ° C and a TUV detector with a detection wavelength of 210 nm and an injection volume of 10 μL. The method can simultaneously determine nine benzene ring organic acids in water, and has a good linear relationship between the concentration of the organic acid peak area and the concentration within a given concentration range. The average recoveries ranged from 79% to 102.8% with RSDs of 0.26% to 5.1% (n = 6). The method is applied to the water samples of each section of a water plant in East Tai Lake and the results are satisfactory.