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色谱  2010 

Determination of 22 antibiotics in environmental water samples using high performance liquid chromatography-electrospray ionization tandem mass spectrometry
高效液相色谱-电喷雾串联质谱法检测环境水样中22种抗生素类药物

Keywords: high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS),solid-phase extraction(SPE),antibiotics,environmental water samples
高效液相色谱-电喷雾串联质谱法
,固相萃取,抗生素类药物,环境水样

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Abstract:

A method for the determination of 22 antibiotics in environmental water samples was developed by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS). The target antibiotics in water samples were enriched and cleaned-up by HLB solid-phase extraction (SPE) cartridges, and then eluted with 6 mL ammonium hydroxide-methanol (5:95, v/v). The eluate was collected and concentrated to 1 mL under a gentle stream of nitrogen gas, and then analyzed by HPLC-ESI MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. The separation was carried out on an XTerra MS C18 column with mobile phases of A, methanol-acetonitrile (1:1, v/v), and B, 0.3% formic acid/water (containing 0.1% ammonium formate, v/v, pH 2.9). The results showed that the average recoveries of antibiotics in tap water and wastewater were 54.9%~130% and 57.4%~138%, respectively, and the corresponding relative standard deviations (RSD, n=3) were 2.85%~28.6% and 2.02%~23.2%, respectively. The method detection limits were 0.05~0.5 ng/L. The developed method was applied to analyze the water samples of Gaobeidian Lake and Xiaoqinghe River in Beijing. The results showed that some antibiotics were detected both in the two samples.

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