摘要
建立了鱼粉中孔雀石绿及其代谢物隐色孔雀石绿残留量的超高效液相色谱-串联质谱仪(UPLC-MS-MS)测定法。样品经乙腈提取,中性Al2O3固相小柱净化,超高效液相色谱C18柱分离,电喷雾正离子多反应模式(MRM)检测,内标法定量。方法的定量限为1.00μg/kg,线性范围为0.25～20.0μg/L。在1.00～20.0μg/kg的加标量下,孔雀石绿平均回收率范围为85.3%～104.4%,隐色孔雀石绿平均回收率范围为85.7%～101.4%,相对标准偏差均小于15%。方法适用于鱼粉样品中孔雀石绿残留的快速检测。
A method was developed for simultaneous determination of malachite green（MG） and leucomalachite green（LMG） residues in fish meal using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry（UPLC-ESI-MS /MS）.Using acetonitrile as an extraction solution,the extract was purified with a neutral alumina solid phase column.Chromatographic separation was achieved using a UPLC C18 column.Electrospray ionization in positive mode,and multiple reaction monitoring（MRM） scan mode and the internal standard method were employed for quantitative analysis.Quantitation limit was 1.00 μg /kg with good linearity ranging from 0.25 to 20.0 μg /L.The average recoveries of MG and LMG spiked at levels of 1.00 ～ 20.0 μg /kg were 85.3% ～ 104.4% and 85.7% ～ 101.4%,respectively,with relative standard deviations（RSD） less than 15%.Due to the advantages of simplicity,rapidity,high accuracy and precision,this method could be suitable for the rapid detection of malachite green residues in fish meal samples.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第8期73-76,共4页
Chinese Journal of Analysis Laboratory
基金
浙江省科技计划项目(2012F30021)
浙江省重点科技创新团队(2010R50028)项目资助
