超高效液相色谱-串联质谱测定水产品中孔雀石绿的含量.docVIP

超高效液相色谱-串联质谱法测定水产品中孔雀石绿残留量 梅光明，郭远明*，陈雪昌，张小军，李佩佩 （浙江省海洋水产研究所, 浙江省海水增养殖重点实验室，舟山 316100） 摘 要：采用超高效液相色谱-串联质谱仪（UPLC-MS-MS）测定水产品中孔雀石绿残留量。该方法经乙腈提取样品，中性氧化铝固相小柱净化，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。方法的定量检出限为0.50 μg·kg-1，线性范围为0.25~20.0 μg·L-1。在0.50~20.0 μg·kg-1的加标浓度下，孔雀石绿回收率范围为80.2 %~104.6%，隐色孔雀石绿回收率范围为85.1%~104.1%，批内和批间试验回收率相对标准偏差均小于8%。方法简便快捷，准确度和精密度高，适用于大批量水产品中孔雀石绿的快速检测。 关键词：水产品；孔雀石绿；隐色孔雀石绿；超高效液相色谱-串联三重四级杆质谱仪 Determination of Malachite Green Residue in Aquatic Products by UPLC-MS-MS MEI Guang-ming, GUO Yuan-ming, CHEN Xue-chang, ZHANG Xiao-jun, LI Pei-pei (Marine Fishery Research Institute of Zhejiang Province,Key lab of Mariculture and Enhancement of Zhejiang province, Zhoushan , 316100, China) Abstract: The residue of malachite green in aquatic product was determined by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). A sample was extracted with acetonitrile, and cleaned up on neutral alumina solid phase column. Chromatographic separation was carried out on UPLC C18 column. The mass spectrometer was performed using multiple reaction monitoring (MRM) with electrespray ionization in positive mode. Quantitation limit was 0.50 μg/kg, with good linearity ranged from 0.25~20.0 μg·L-1. Average recoveries spiked at the levels from 0.50~20.0 μg·kg-1 were 80.2%~104.6% for malachite green, 85.1%~104.1% for leucomalachite green, and relative standard deviations both for intra- and inter- test were less than 8% .With the advantages of simplicity, rapidity, high accuracy and precision, this method could be suitable for the rapid detection of malachite green in in large quantities of aquatic products. Key words: Aquatic Product; Malachite Green; Leucomalachite Green; UPLC-MS-MS 孔雀石绿属于一种工业染料，在水产养殖中经常用来治疗水霉病、腮霉病以及环境的消毒等[1]。研究表明孔雀石绿及其代谢产物隐色孔雀石绿在动物体内消除缓慢，残留时间长，且具有致癌、致畸和致突变作用[2-3]，欧美很多国家以及我国农业部公告第235号文件都将孔雀石绿列为禁止使用药物，规定在动物源性食品中不得检出[4]。目前孔雀石绿的检测标准主要有高效液相色谱法[5]和液质联用法[6]。高效液相色谱法存在前处理复杂、需要衍生化、回收率不高和易出现假阳性等缺点。液质联用法由于前处理简单，对物质定性定量分析准确可靠，回收率高，因此在孔雀石绿的测定过程中获得了广泛的应用