| 摘要: |
| [摘 要]：建立了快速超高效液相色谱-串联质谱(UPLC- MS/MS)测定猪肉样品中新型兽药盐酸沃尼妙林残留的检测确证方法。样品使用乙腈提取，在提取过程中同时加入正己烷去除脂质杂质，离心后取乙腈提取液，浓缩至干，用1ml 0.1%甲酸水:乙腈（60:40 V:V）复溶上机。以反相C18柱作为分离柱，以 0.1%甲酸乙腈和0.1%甲酸水为流动相，进行梯度洗脱。方法的线性范围：10μg/kg~500μg/kg，定量限为10μg/kg，检出限为20μg/kg，在三个浓度水平（20μg/kg、50μg/kg和100μg/kg）下进行添加实验，回收率为88.04%~102.9%，批内相对标准偏差为1.3%~6.5%，批间相对标准偏差为3.0%~4.6%。表明此方法简便迅速且稳定有效，适合快速检测猪肌肉中的沃尼妙林残留。 |
| 关键词: 沃尼妙林 超高效液相色谱串联质谱 猪肉残留检测 |
| DOI： |
| 投稿时间：2010-07-19修订日期：2010-08-22 |
| 基金项目: |
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| Detection of valnemulin residues in pork by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry |
| Yu Qianqian |
| (College of Veterinary Medicine in China Agriculture University) |
| Abstract: |
| A method is described for the quantitative and qualitative determination of Valnemulin (VLM) Hydrochloride residue in porcine by using Ultra performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile at the same time added hexane to remove the fat, then centrifuged and removed the hexane, just evaporated the part of acetonitrile. The residue was dissolved with acetonitrile-0.1% formic acid (40:60 V: V). Chromatographic separation of the Valnemulin is performed on a C18 column using formic acid 0.1% in acetonitrile and formic acid 0.1% in water by gradient elution. This method has good linearity over concentration range of 10μg/kg~500μg/kg. The LOD and LOQ were 10μg/kg and 20μg/kg respectively. Average analyte recoveries were from 88.04% to 102.9% in replica sets of porcine in three different concentrations: 20, 50, 100μg/kg. Inter-day RSD is from 1.3% to 6.5%, and intra-day RSD is from 3.0% to 4.6%. These results suggested that this method was a robust and effective method for the determination of valnemulin residues in pork. |
| Key words: valnemulin UPLC-MS/MS porcine residue |
