液相色谱串联质谱法检测水产品硝基呋喃类代谢物的改进  

Improved Liquid Chromatography-Tandem Mass Spectrometric Method for Determination of Nitrofuran Metabolites Residues in Aquatic Products

作　　者：刘四新[1] 胡先娥[1] 林正峰[2] 何雪莲[2] 刘红专[2] 李从发[1] 

机构地区：[1]海南大学食品学院,海南海口570228 [2]海南出入境检验检疫局技术中心,海南海口570311

出　　处：《食品科学》2009年第20期331-335,共5页Food Science

基　　金："十一五"国家科技支撑计划项目(2007BAD76B06)

摘　　要：国标GB/T20752—2006测定水产品硝基呋喃类药物代谢物的实际回收率为40%左右、线性范围0.2～2μg/kg。为改进不足,本实验改用乙酸乙酯提取、液液萃取净化,并适当改变LC-MS/MS检测中液相色谱条件和质谱条件,结果显示,样品前处理时间大大缩短,方法回收率81.3%～106.0%,相对标准偏差小于11%,线性范围0.1～4.0μg/kg,相关系数0.999以上,最低检出限0.1μg/kg。改进后的方法比国标方法在准确度、灵敏度和稳定性等方面均有所提高。The Chinese national standard method, GB/T 20752 -- 2006 has been used for the determination of nitrofuran metabolites residues in aquatic products using liquid chromatography-tandem mass spectrometry （LC-MS/MS）, with a recovery rate of 40% and a linear range of 0.2-2 μg/kg. Extraction of test portions with ethyl acetate followed by clean-up using liquidliquid extraction was adopted and appropriate adjustments of LC-MS/MS conditions were conducted as improvements for the method. Results showed that the pretreatment time was shortened, and the average spike recovery rates for six replicate determinations were elevated to 81.3% - 106.0%, with a RSD of less than 11%. This method exhibited a linear range of 0.1 - 4 μ g/kg （r^2 〉 0.999） and a limit of detection of 0.1 μg/kg.

关 键 词：硝基呋喃类药物代谢物 液相色谱串联质谱法 水产品 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]