分散固相萃取结合液相色谱串联质谱法检测牛可食性组织中泰地罗新残留量

Determination ofTildipirosin in Edible Bovine Tissues by Dispersive Solid Phase Extraction Combined with Liquid Chromatography- Tandem Mass Spectrometry

关键词:  泰地罗新  分散固相萃取  串联质谱法

Key words:  Tildipirosin  dispersive solid phase extraction  Tandem mass spectrometry

摘要:

建立了分散固相萃取结合液相色谱串联质谱法检测牛肉、牛脂肪、牛肝和牛肾等可食性组织中的泰地罗新残留量的方法。取牛组织样品经50%(v/v)乙腈溶液提取,加入无水硫酸镁和氯化钠进行脱水和盐析,正己烷脱脂,高速离心分层后,取适量乙腈层溶液经0.1%(v/v)甲酸稀释后,用酸性氧化铝粉末进行样品净化并以10000 r/min离心取上清液,过0.22 μm滤膜后上机测定。使用反相色谱柱进行分离,流动相为0.1 %甲酸和乙腈溶液,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,方法的最低检测限为5 μg/kg,最低定量限为10 μg/kg,在10μg/kg~1000μg/kg范围内线性关系良好(r >0.995),添加回收率在60 %～110 ％,RSD＜10 ％,表明该方法具有较好的准确度与精密度。

Abstract:

To determine residue of tildipirosin in edible bovine tissues such as muscle, fat, liver and kidney, a dispersive liquid 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. After high speed centrifugation,the extract was diluted by the 0.1%(v/v) formic acid and purified by the acid alumina powder. After 10000 r/min centrifugation, the extract was filtered by 0.22 μm film and then injected. 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 mass spectrometry. The results showed that the LOD of the method was 5 μg/kg and the LOQ was 10 μg/kg. The linearity of the method was good in the range of 10 ~ 1000μg/kg and the liner correlations were all above 0.995, the recovery were between 60 % ~ 110 ％, and the RSD were lower than 10 %, which showed the good accuracy and precision of the method.