固相萃取-羟基衍生化-气相色谱/质谱联用测定滇池水体中酚类内分泌干扰物

DETERMINATION OF PHENOLS IN SUFACE WATER OF DIANCHI LAKE BY SOLID EXTRACTION-HYDROXYL DERIVATIZATION-GC/MS

采用PTA-OH为衍生化试剂,对酚类内分泌干扰物的衍生化条件进行了优化,并在优化条件下,利用固相萃取-羟基衍生化-气相色谱/质谱法检测了滇池水体中酚类内分泌干扰物的浓度.结果表明,目标物PTA-OH衍生化在乙酸乙酯中、20℃条件下衍生化5min可达到最佳衍生化效果,衍生化后酚类内分泌干扰物的GC/MS检测限达到0.1pg.μl-1,检测范围为20—1000pg.μl-1;滇池水体中的辛基酚的浓度为ND—56.5ng.l-1;枯烯基酚的浓度为23.5—48.5ng.l-1;壬基酚的浓度为13.6—141.6ng.l-1;双酚A的浓度为ND—4713.6ng.l-1.滇池水体中4种酚类内分泌干扰物普遍存在,其中双酚A的污染较严重.

Phenyltrimethylammonium （PTA-OH） was used to derivatize phenolic endocrine disrupting chemicals （EDCs） and its derivatization conditions were tested. The optimized derivatization conditions were then used in a solid phase extraction-hydroxyl derivatization-GC/MS method for simultaneous determination of target phenols in surface water of Dianchi Lake. The results showed that the optimum derivatization conditions for derivatization with PTA-OH were ethyl acetate as solvent at 20℃ for 5min,and the instrumental detection limits for phenolic EDCs after derivatization was found to be 0.1pg·μl^-1 with a linear detection range from 20 to 1000pg·μl^-1. The concentrations of 4-tert-octylphenol （4-t-OP）,4-cumylphenol （4-CP）,4-nonylphenol （4-NP） and bisphenol A （BPA） in surface water of Dianchi Lake were ND—56.5ng·l^-1,23.5—48.5ng·l^-1,13.6—141.6ng·l^-1 and ND—4713.6ng·l^-1,respectively.This indicates the four phenolic EDCs are ubiquitously present in surface water of Dianchi Lake,among which BPA is dominant one.