分散固相萃取法结合液相色谱串联质谱法检测鸡可食性组织中泰万菌素及3-乙酰泰乐菌素残留量

Determination of Aivlosin and 3-Acetyl Tylosin in Edible Chicken Tissues by Dispersive Solid Phase Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

建立了检测鸡肉、鸡皮脂、鸡肝和鸡蛋中泰万菌素以及其主要代谢产物3-乙酰泰乐菌素残留量的液相色谱串联质谱方法。前处理使用分散固相萃取法,选择使用50%(V/V)乙腈提取,无水MgSO_4进行脱水和盐析,正己烷脱脂,酸性氧化铝粉末进行样品净化。将离心后的上清液以如下方法进行上机检测:使用反相色谱柱进行分离,流动相为0.1%甲酸和乙腈,采用梯度程序进行洗脱,三重四级杆质谱进行定性定量分析。实验结果表明,方法的最低检出限为2.5μg/kg,最低定量限为5μg/kg,在5~200μg/kg范围内线性关系良好(r>0.995),添加回收率在60%~110%,RSD<20%,表明该方法具有较好的准确度与精密度。

To determine residue of tylvalosin （TLV） and 3-acetyl tylosin （3-AT） in edible chicken tissues such as muscle, skin/fat, liver and egg, a dispersive solid phase extraction method was used to process the sample. The 50%（V/V） acetonitrile was chosen to extract the target compounds, the anhydrous magnesium sulfate was chosen to dehydrate and salt out, the n-hexane was chosen to degrease and the acid alumina powder were chosen to purify the sample. After centrifugatiou, the extract was determined by the method below. The targets was separated by the gradient elution with a reverse phase column as the stationary phase and 0.1% formic acid with acetonitrile as the mobile phase. The qualification and quantification were achieved by a tandem massspectrometry. The results showed that the LOD of the method was 2.5 I^g/kg and the LOQ was 5 linearity of the method was good in the range of 5 - 200 μg/kg and the liner correlations were all above the recovery of 7 targets were between 60% and 110%, and the RSD were lower than 20%, which good accuracy and precision of the method μg/kg. The 0.995, and showed the