超高效液相色谱-电喷雾串联质谱法测定饲料中残留的三聚氰胺

饲料样品经1%三氯乙酸-二甲基亚砜提取,Waters Oasis MCX柱净化,超高效液相色谱分离,最终采用电喷雾串联四极杆质谱进行检测。结果表明,三聚氰胺在饲料中的含量范围为10～5000 μg/kg时,线性关系良好(r＞0.99)。在10～100 μg/kg 的添加水平范围内的平均回收率为83%～94%,相对标准偏差为4.2%～6.5%。该方法的检出限为10 μg/kg。

Determination of melamine residue in feeds by ultra performance liquid chromatography coupled with electrospray tandem mass spectrometry

A method for fast determination melamine residue in feeds was established. An ultra performance liquid chromatography coupled with electrospray ionization quadrupole tandem mass spectrometry (UPLC-ESI-MS/MS) was used. The residue was quantified with multiple reaction monitoring (MRM) mode. The method was validated and good results were obtained with respect to precision, repeatability and spiked recovery. The limit of detection was 10 microg/kg for melamine, and the linear range was from 10 to 5 000 1g/kg. The average recoveries were between 83% and 94% in the spiked range of 10 - 100 microg/kg, and the relative standard deviations (RSDs) were between 4.2% and 6.5%. The method has good repeatability and high sensitivity, and can be applied for the determination of melamine residue in feeds.