超高效液相色谱-质谱联用检测土壤中两种抗生素呋喃唑酮和氟苯尼考  

Determination of Furazolidone and Florfenicol in Soil by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：南琼 唐景春[1,2,3] 何若竹 胡羽成 吴涛 

机构地区：[1]南开大学环境科学与工程学院,天津300071 [2]环境污染过程与基准教育部重点实验室,天津300071 [3]天津市城市环境污染诊断与修复技术工程中心,天津300071 [4]天津市水利科学研究院,天津300061

出　　处：《分析化学》2017年第11期1600-1605,共6页Chinese Journal of Analytical Chemistry

基　　金：水体污染控制与治理科技重大专项(No.2015ZX07203-011-06);天津市水务局局科研项目(No.KY2015-01);863成果转化项目(No.14RCHZSF00144)资助

摘　　要：建立了超高效液相色谱-串联质谱(UPLC/MS/MS)检测土壤中多种环境基质下呋喃唑酮和氟苯尼考的方法。提取液采用磷酸盐缓冲溶液(p H=3)-乙腈(3∶7,V/V),经过SPE固相萃取小柱SAX-HLB串联富集,使用Waters BEH C18色谱柱(2.1×100 mm)进行分离,UPLC/MS/MS在多反应监测模式下进行定性与定量分析。以3倍信噪比确定方法检出限,以10倍信噪比确定方法定量限。结果表明,本方法在5 min内即可分离两种物质,呋喃唑酮和氟苯尼考的检出限分别为1.19和0.41μg/kg;定量限分别为3.40和1.37μg/kg。50μg/L加标水平的呋喃唑酮和氟苯尼考的回收率分别为92%和79%;200μg/L加标水平下呋喃唑酮与氟苯尼考的回收率分别为96%和86%。A detection method for furazolidone and florfenicol in soil with various environmental matrices was established using ultra performance liquid chromatography-tandem spectrometry（ UPLC/MS/MS） technique.Extracting solution of a mixture of phosphate buffer（ p H = 3） and acetonitrile（ 3 ∶ 7,V/V） was used in this experiment. The extracted water samples were enriched by SAX-HLB solid phase extraction column before the process of nitrogen blowing（ high purity nitrogen）. The enriched antibiotics were desalted with 8 m L of methanol. Waters BEH C18（2.1 × 100 mm） column was used for the sample separation. UPLC/MS/MS was carried out for qualitative and quantitative analysis under multi-reaction monitoring mode. The detection limit of the method was determined by 3 times of signal-to-noise ratio,and the limit of determination of the method was determined by 10 times of signal-to-noise ratio. The results showed that the detection limits of furazolidone and florfenicol were 1. 19 and 0. 41 μg/kg,respectively,and the limits of quantitation of furazolidone and florfenicol were 3. 40 and 1. 37 μg/kg,respectively. Besides,recovery experiment showed that,for the soil samples spiked with 50 μg/L furazolidone and florfenicol,the recoveries were 79% for florfenicol and 92% for furazolidone. Similarly,for the soil samples spiked with 200 μg/L furazolidone and florfenicol,the recoveries were 96% for furazolidone and 86% for florfenicol.

关 键 词：超高效液相色谱-串联质谱 呋喃唑酮 氟苯尼考 固相萃取 

分 类 号：O657.63[理学—分析化学]