液相色谱串联质谱法正负模式切换同时检测饲料中10种硝基呋喃类化合物

Determination of 10 Nitrofurans in Feed by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Positive and Negative Switching

关键词:  10种硝基呋喃药物  正负模式切换  串联质谱法

Key words:  10 nitrofurans  positive and negative switching  Tandem mass spectrometry

摘要:

建立了超高效液相色谱-串联四级杆质谱法检测饲料中的10种硝基呋喃类化合物的方法。2g饲料样品经0.1 mol/mL HCl : 乙腈=1:1提取,9000 RPM高速离心后稀释,经酸性氧化铝粉末净化后进样分析。采用Thermo Hypersil Gold C18色谱柱(150 mm×2.1 mm, 1.9 μm)作为固定相,0.1 %甲酸和乙腈作为流动相进行梯度洗脱。质谱采用正负离子切换同时扫描,SRM模式进行分析。10种硝基呋喃类化合物在最优化条件下分离良好,在定量范围内均线性良好(线性相关系数r≥0.99),回收率也可达到63.2 % ～ 89.7 % ,相对标准偏差(RSD)小于9.3 %。本方法具有简便、快速、灵敏、准确等特点,适用于饲料中违法添加硝基呋喃类化合物的检测。

Abstract:

To determine the illegal added 10 nitrofuranes in feed, a high performance liquid chromatography –tandem quadrupole mass spectrometry method was established. 2g feed was extracted by 0.1 mol/mL HCl : acetonitrile =1:1. The extraction was centrifuged under 9000 RPM and purified by acid then diluted to inject. Thermo Hypersil Gold C18 column (150 mm×2.1 mm, 1.9 μm) was chosen to be the solid phase and 0.1 % formic acid combined with acetonitrile were chosen to be the liquid phase to achieve the grad elution. The mass spectrometer was operated using positive and negative switching under SRM mode. Under the optimal conditions, 10 nitrofuranes were separated well, Good linearity was obtained in their respective quantitative range (correlation coefficients r≥0.99 ). The average recoveries were in the range of 63.2 % -89.7 % and the relative standard deviations (RSD) were lower than 9.3%. The method was proved to be convenient, economical, sensitive and accurate. The research was proved to be effective for the detemination of the illegal added 10 nitrofuranes in feed.