| 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。 |
| 关键词: 泰地罗新 分散固相萃取 串联质谱法 |
| DOI： |
| 投稿时间：2018-12-28修订日期：2019-02-15 |
| 基金项目:上海市科技兴农重点攻关项目[No. (2016)3-2] |
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| Determination ofTildipirosin in Edible Bovine Tissues by Dispersive Solid Phase Extraction Combined with Liquid Chromatography- Tandem Mass Spectrometry |
|
| (Shanghai Municipal Supervisory Institute Veterinary Drugs and Feedstaff) |
| 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. |
| Key words: Tildipirosin dispersive solid phase extraction Tandem mass spectrometry |
