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

发布时间：2018-03-28 05:16

本文选题：超高效液相色谱-串联质谱　切入点：呋喃唑酮　出处：《分析化学》2017年11期

【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%。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (UPLC / MS / MS) method was established for the detection of furazolidone and florfenicol under various environmental substrates in soil. The extraction solution was enriched by SPE solid-phase extraction column SAX-HLB series with phosphate buffer solution of 3: 7V / VN. The Waters BEH C18 column (2.1 脳 100mm) was used for qualitative and quantitative analysis of UPLC / MS / MS in multi-reaction monitoring mode. The detection limit was determined by the method of 3 times SNR and the quantitative limit was determined by 10 times SNR. In this method, two substances can be separated within 5 min. The detection limits of furazolidone and florfenicol were 1.19 and 0.41 渭 g / kg, respectively, and the recoveries of furazolidone and florfenicol were 92% and 79 渭 g / L, respectively, and the recoveries of furazolidone and florfenicol were 96% and 86% at the standard level of 3.40 渭 g / L and 1.37 渭 g / L, respectively.
【作者单位】：南开大学环境科学与工程学院;环境污染过程与基准教育部重点实验室;天津市城市环境污染诊断与修复技术工程中心;天津市水利科学研究院;
【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
【分类号】：O657.63;X833

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