液相色谱串联质谱法测定阿维菌素残留仪器条件的优化

样品提取净化过程建立在SN/T1973-2007《进出口食品中阿维菌素残留量的检测方法液相色谱-串联质谱法》基础上,用乙腈提取,中性氧化铝固相萃取柱净化,外标法定量。Waters2695-TQD电喷雾正离子(ESI+)多反应检测,通过优化锥孔电压(Cone(V)),碰撞能量(Collision),流动相,定容液比例进行了优化。结果表明:锥孔电压为22,阿维菌素能形成稳定的M+NH4+峰,碰撞能量为25,能形成稳定的碎片离子,并且阿维菌素在0.005~0.25mg/kg范围内保持良好线性范围(R20.999),回收率76.3%~101.8%之间,检出限为0.005mg/kg,符合痕量分析要求并能满足确证需要。

Optimization of Instrument Conditions in Determination of Abamectin Residues by LC/MS/MS Spectrometry

Sample extraction and purification process was based on SN/T1973-2007 《the import and export of abameetin residues in food detection method liquid chromatography-tandem mass spectrometry》, extracted with acetonitfile, neutral alumina solid-phase extraction column pu- rification, external standard quantitation. Waters2695-TQD positive ions electrospray （ESI＋） multiple reaction monitoring, by optimizing the taper hole （Cone voltage （V）） and Collision energy （Collision）, mobile phase and filling volume liquid ratio is optimized. The results showed that： when taper hole voltage is 22, Abamectin can form stable M＋NH4∽ peak; when the colli- sion energy was 25, it can form stable fragmentions. Abamectin in the concentration of 0.005- 0.25mg/kg the method maintains good linear range （R2〉0.999） with recovery 76.3%-101.8% and detection limit O.O05mg/kg, which can meet the requirements of trace analysis validation.