液相色谱串联质谱法快速同时测定废水中的14种磺胺类药物
Rapid simultaneous determination of 14 sulfonamides in wastewater by liquid chromatography tandem mass spectrometry.
作者信息
Ye Sai, Yao Ziwei, Na Guangshui, Wang Juying, Ma Deyi
机构信息
Coastal Ecology Key Laboratory of State Oceanic Administration, National Marine Environmental Monitoring Center, Dalian, China.
出版信息
J Sep Sci. 2007 Oct;30(15):2360-9. doi: 10.1002/jssc.200600539.
This paper describes a rapid method for the determination of 14 kinds of sulfonamides (SAs) in wastewater using SPE, and LC-MS/MS with positive ESI (ESI(+)) and selected reaction monitoring (SRM) mode. The SPE was performed on an Oasis hydrophilic-lipophilic-balanced (HLB) cartridge. Chromatographic separation on a C18 column was achieved using a binary eluent containing methanol and water with 0.2% formic acid. Typical recoveries of the analytes ranged from 22.3 to 87.0% at a fortification level of 100 ng/L. The LODs in wastewater except sulfathiazole (3 ng/L) could be detected and quantified at levels as low as 1 ng/L. Finally, the method was applied to water from the municipal outlet and the aquaculture wastewater effluent. Sulfamethazine (SM(2)), sulfamethoxypyridazine (SMP), and sulfamethoxazole (SMZ) were most frequently found in wastewater in a concentration range between 1.2 and 31.7 ng/L.
本文描述了一种使用固相萃取（SPE）以及采用正离子电喷雾电离（ESI(+)）和选择反应监测（SRM）模式的液相色谱-串联质谱（LC-MS/MS）快速测定废水中14种磺胺类药物（SAs）的方法。SPE在Oasis亲水亲脂平衡（HLB）柱上进行。在C18柱上进行色谱分离，使用含有甲醇和0.2%甲酸的水的二元洗脱液。在100 ng/L的加标水平下，分析物的典型回收率为22.3%至87.0%。除磺胺噻唑（3 ng/L）外，废水中的检测限低至1 ng/L时即可检测和定量。最后，该方法应用于城市排水口和水产养殖废水排放口的水样。二甲氧苄氨嘧啶（SM(2)）、磺胺甲氧嗪（SMP）和磺胺甲恶唑（SMZ）在废水中最常被检测到，浓度范围在1.2至31.7 ng/L之间。
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