污泥中氟喹诺酮类微污染物的测定方法研究  

Improved determination of three fluoroquinolones in sewage sludge

作　　者：王洋[1] 杨雪玲[1] 易玲 丁小双 钟懿 于洁[1] 王侃[1] 莫春阳 WANG Yang;YANG Xueling;YI Ling;DING Xiaoshuang;ZHONG Yi;YU Jie;WANG Kan;MO Chunyang(School of Civil and Environmental Engineering,Ningbo University,Ningbo 315211,China;Ningbo Zhongke Testing Technology Service Co.,Ltd.,Ningbo 315105,China;Sanmenxia Chunhe Building Materials Co.,Ltd.,Sanmenxia 472135,China)

机构地区：[1]宁波大学土木与环境工程学院,浙江宁波315211 [2]宁波中科检测技术服务有限公司,浙江宁波315105 [3]三门峡市春和建材有限公司,河南三门峡472135

出　　处：《宁波大学学报（理工版）》2021年第3期60-65,共6页Journal of Ningbo University：Natural Science and Engineering Edition

基　　金：国家自然科学基金(51408325).

摘　　要：污泥中累积了高浓度的氟喹诺酮类(Fluoroquinolones,FQs)有机微污染物,对生态环境和人类健康潜在危害巨大.本文对污泥中氧氟沙星(Ofloxacin,OFL)、诺氟沙星(Norfloxacin,NOR)、环丙沙星(Ciprofloxacin,CIP)3种FQs的固相萃取-液相色谱分析方法进行优化研究.结果表明,污泥经EDTA-Na_(2)、磷酸盐溶液-乙腈混合液(1:1,pH=3)超声提取两次,提取液经HLB固相萃取柱富集纯化,甲醇和碱性甲醇洗脱,洗脱液经氮吹浓缩后,污泥中FQs的回收率较高.液相色谱测定流程经优化后为C18色谱柱为分离柱、甲醇/水溶液为流动相进行梯度洗脱,荧光检测器检测.色谱图中OFL、NOR、CIP具有较好的分离效果,污泥中OFL、NOR、CIP回收率为48.1%~53.4%.High concentration of fluoroquinolones antibiotic has been detected in the sewage sludge,posing great hazards to the environment and human health.An improved solid phase extraction and liquid chromatography method was developed for the determination of ofloxacin(OFL),norfloxacin(NOR),and ciprofloxacin(CIP)in the sludge.The OFL,NOR,and CIP were extracted two times from the sludge by sonication with EDTA-Na_(2) and phosphate solution/acetonitrile(1:1,pH=3).The extract was purified using HLB solid phase extraction column,eluted with methanol and alkaline methanol,and concentrated by nitrogen blowing,followed by liquid chromatography determination.The liquid chromatography was equipped with a C18 column and a fluorescence detector,with methanol and pure water as mobile phase for gradient elution.The OFL,NOR,and CIP in the sludge were well extracted and separated with recoveries of 48.1%-53.4% by the developed method.

关 键 词：污泥 氟喹诺酮类 固相萃取 液相色谱 

分 类 号：X708[环境科学与工程—环境工程]