在线固相萃取-液相色谱-四极杆/飞行时间质谱法快速筛查水体中60种有机毒物

Rapid screening and confirmation of 60 organic contaminants in water by online solid phase extraction and liquid chromatographyquadrupole/time-of-flight mass spectrometry

采用在线固相萃取-液相色谱-四极杆/飞行时间质谱(online SPE-LC-QTOF)对水体中农药、激素和抗生素等60种有机毒物进行快速筛查、定性识别和准确定量.样品经在线固相萃取小柱萃取吸附后,被流动相反冲出萃取小柱,进入C18色谱柱进行分离,正、负离子模式分别扫描测定.结果表明,60种化合物在一定浓度范围内呈良好的线性相关性,相关系数均大于0.998.各目标物的方法检出限为0.2—4.8 ng·L-1,在低、中、高的3个添加水平下,各化合物的平均回收率为70.5%—129%,相对标准偏差为1.4%—15.4%.该方法利用自建标准谱库检索,实现有机毒物的快速筛查,并使用二级特征碎片离子进行确证,具有快速高效等优点.太湖流域水体筛查结果阐明了太湖流域新型污染物的分布状况和污染规律.

A method for the rapid screening,qualitative confirmation and quantification of 60organics including pesticides,hormones and antibiotics in water was developed by online solid phase extraction and liquid chromatography-quadrupole/time-of-flight mass spectrometry（online SPE-LC-QTOF）.The samples were adsorbed to the online SPE column,back-flushed into LC system with the mobile phase and separated on a C_（18）column.The target compounds were monitored in both positive and negative full scan modes.All the compounds had the good linearity within their respective linear ranges（r〉0.998）.The limits of detection（LODs）were 0.2—4.8 ng·L^（-1）.The method validation was carried out at three spiked levels,and the recoveries were 70.5%—129%with the relative standard deviations（RSDs）of 1.4%—15.4%.The screening of analytes was performed by library searching and the secondary fragment ion spectra were employed for the confirmation.This method is fast and efficient.The results illustrate the distribution and pollution of the new pollutants in the Taihu Lake.