漂浮液滴固化分散液液微萃取与高效液相色谱联用检测环境水样中的3种烷基苯酚

Dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by high performance liquid chromatography for the determination of three alkylphenols in environmental water samples

建立了漂浮液滴固化分散液液微萃取(DLLME-SFO)方法,以脂肪酸作为萃取剂,以甲醇作为分散剂,与高效液相色谱联用检测了环境水样中3种烷基苯酚。对影响前处理方法的因素进行了详细考察,在最佳萃取条件(60μL萃取剂辛酸、600μL分散剂甲醇、pH值为2.0~8.0、10 mL水样中加入0.5 g NaCl)下,3种烷基苯酚在20~1 500μg/L范围内具有良好的线性关系,相关系数不小于0.998 5,3种目标化合物的检出限为0.45~0.61μg/L,富集倍数为145~169,实际样品中3个水平的加标回收率为80.1%~109.9%。该方法将脂肪酸作为萃取剂,与HPLC联用实现了烷基苯酚的富集与检测,为环境水样中烷基苯酚的检测提供了对环境友好的前处理新方法。

A simple,rapid and eco-friendly method named dispersive liquid-liquid microextrac-tion based on solidification of floating organic drop （DLLME-SFO） was developed for the deter-mination of 2-tert- butyl-4-ethylphenol, 4-tert-octylphenol and 2,4-di-tert-butylphenol inwastewater samples coupled with high performance liquid chromatography-ultraviolet detection （HPLC-UV）. Octanoic acid was served as extraction solvent,and methanol was selected as dis-persive solvent. The parameters affecting the extraction efficiency including the type and vol-ume of the extraction solvents and the dispersive solvents,the pH and the salt addition were optimized. Under optimum conditions,the linear range was 20-1 500 p^^L for all the three tar-get alkylphenols. Limits of detection （LODs, S/N =3） were in the range of 0.45-0.61 p^^L. The enrichment factors （EFs） varied from 145 to 169,and the recoveries at three spiked levels were in the range of 80. 1% -109. 9%. It demonstrated that fatty acids including octanoic acid and nonanoic acid could be used as extraction solvent in DLLME-SFO method. The method is suitable for the determination of alkylphenols in environmental water samples.