摘要
本文通过优化固相萃取条件、色谱分离条件、质谱检测参数,建立一种同时测定水中磺胺类、四环素类、大环内酯类、喹诺酮类等抗生素的同位素内标稀释高效液相色谱质谱法.研究表明,通过特征离子和色谱保留时间进行定性,可以同时准确分辨多种抗生素;检测方法具有较好的灵敏度(方法定量限为2—50 ng·L^(-1))和精密度(日内和日间相对标准偏差分别为1.3%—4.8%和3.0%—9.8%),方法回收率为43%—112%.该方法应用于检测珠江水系的河水样品,所检样品中均含有不同含量的多种抗生素,特别是磺胺类、大环内酯类等常用药物,表明这些河水已受到了一定的抗生素污染.
In this work,simultaneous determination of sulfonamides,tetracyclines,macrolids and fluoroquinolones in water by isotope-diluted high performance liquid chromatography-mass spectrometry was established. Solid phase extraction conditions,chromatographic separation and mass spectrometric parameters were optimized. It was revealed that the antibiotics were qualified using the characteristic ions and retention time. Method quantification limits were in the range of 2—50 ng·L^-1. Intraday and interday precision values were in the range of 1. 3%—4. 8% and 3. 0%—9.8%,respectively. Spiking recovery was within 43%—112%. The method was applied to determine the antibiotics in water samples of Pearl River. Most antibiotics, especially sulfonamides and macrolids,were detected,revealing that the water was contaminated to some extent.
出处
《环境化学》
CAS
CSCD
北大核心
2016年第7期1493-1499,共7页
Environmental Chemistry
基金
广东省省级科技计划项目(2016A040403039)
工业和信息化部电子第五研究所发展基金(12Q01)
广东省自然科学基金(2014A030310141)资助~~
关键词
抗生素
高效液相色谱质谱法
河水
固相萃取
同位素内标稀释法
antibiotics
high performance liquid chromatography
river water
solid phase extraction
isotope-diluted