兔可食性组织中杆菌肽残留量HPLC-MS/MS测定方法

建立兔可食性组织中杆菌肽残留标志物的HPLC-MS/MS检测方法.兔可食性组织(肌肉、脂肪、肝脏和肾脏)中杆菌肽残留用0.5％三氟乙酸水提取,10％三氯乙酸乙腈沉淀蛋白,正己烷除脂,HLB 150 mg固相萃取柱净化,以0.1％甲酸水和乙腈(0～0.5 min 15％乙腈,7.5～8.0 min 85％乙腈,8.1～1...

Determination of Bacitracin residues in rabbit edible tissue by HPLC-MS/MS

(Objective)A high performance liquid chromatography-tandem mass spectrometry method was established for determining of bacitracin residues in rabbit tissues. (Method)The rabbit tissue samples (muscle, fat, liver and kidney) were extracted with 0.5% trifluoroacetic acid water, precipitated with 10%acetonitrile trichloroacetate, hexane removed fat, and purified with HLB 150mg solid-phase extraction column. Gradient elution was conducted with 0.1% formic acid water and acetonitrile (0-0.5min 15% acetonitrile, 7.5-8.0min 85% acetonitrile, 8.1-10.0min 15% acetonitrile) as the gradient elution. Electrospray ion source (ESI), positive ion mode and MRM mode were used in mass spectrometry. (Result)The results showed that the linear relationship between the concentration and response value of bacitracin was good in the concentration range of 50~1000ng/g (calculated by bacitracin), and the correlation coefficient was greater than 0.99. The detection limit of the method was 30ng/g, and the quantitative limit was 50ng/g. The average recovery rate of bacitracin was 74.7%~ 83.8 % the relative standard deviations below 10%.(Conclusion)The method developed in this study can meet the requirements of detection of residual bacitracin in rabbit tissue.