QuEChERS结合高效液相色谱-串联质谱法测定饲料中氯霉素

    Determination of Chloramphenicol in Feed by QuEChERS Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 建立QuEChERS结合高效液相色谱-串联质谱法测定饲料中氯霉素方法。样品经水相分散后用乙腈提取,经QuEChERS方法净化后,采用高效液相色谱-串联质谱法测定,外标法定量。以超纯水和甲醇作为流动相,用Hypersil GOLD C18色谱柱(1.9 μm,2.1 mm×100 mm)进行梯度洗脱,采用电喷雾离子源(ESI-)、负离子扫描多反应监测(MRM)模式进行定性和定量分析。结果表明:氯霉素在5.0~200.0 ng·mL-1的范围内线性关系良好(r=0.999 2)。在10.0、20.0、50.0 μg·kg-1添加水平下的回收率为84.2%~89.7%,相对标准偏差(n=6)为6.5%~8.8%,检出限(以信噪比>3计)为0.2 μg·kg-1,定量限(以信噪比>10计)为0.6 μg·kg-1。该方法精密度好,灵敏度高,能简便地准确测定饲料中的氯霉素。

       

      Abstract: This study aimed to establish a method for the determination of chloramphenicol in feed by using QuEChERS combined with the high performance liquid chromatography-tandem mass spectrometry method. After water dispersion, the samples were extracted with acetonitrile. And then after the purification by QuEChERS method, the samples were determined by high performance liquid chromatography-tandem mass spectrometry and quantified by external standard method. By using the ultrapure water and methyl alcohol as mobile phases, the gradient elution was carried out by Hypersil GOLD C18 column (1.9 μm, 2.1 mm×100 mm). And then the qualitative and quantitative analysis was carried out by using the electrospray ionization (ESI-) and anion scanning multiple reaction monitoring (MRM) modes. The results showed that the linear relation of chloramphenicol was good in the range of 5.0-200.0 ng·mL-1 (r=0.999 2). The recoveries at the adding levels of 10.0, 20.0 and 50.0 μg·kg-1 ranged from 84.2% to 89.7%, the relative standard deviations (n=6) were 6.5%-8.8%, the limits of detection (based on S/N>3) were 0.2 μg·kg-1, and the limits of quantitation (based on S/N>10) were 0.6 μg·kg-1. The method had good precision, high sensitivity and could be used to determine the chloramphenicol in feed simply and accurately.

       

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