超高效液相色谱-串联质谱法同时快速筛查检测食品中的10种抗凝血类鼠药  

Rapid simultaneous screeningand detection of ten anticoagulant rodenticides in foods byultra-highperformance liquid chromatography-tandem mass spectrometry

作　　者：朱峰[1] 刘华良[1] 陈蓓[1] 荣维广[1] 马永建[1] 

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009

出　　处：《色谱》2013年第5期473-476,共4页Chinese Journal of Chromatography

基　　金：卫生部公益性行业科研专项项目(200902009);江苏省科技厅科技支撑计划项目(BE2010745);江苏省"十二五"科教兴卫工程项目(ZX201109)

摘　　要：创建了一种利用超高效液相色谱－串联质谱同时快速筛查检出食品中10种抗凝血类鼠药的方法。试样用乙腈提取．QuEChERS净化，以5mmol／L乙酸铵和乙腈为流动相进行梯度洗脱，经Poroshell 120EC-C18柱（100mm×2．1mｍ．2．7μm；美国Agilent公司）分离，采用电喷雾电离（ESI）负离子质谱在多反应检测（MRM）模式下检测。10种鼠约均在5～500μg／L范围内呈现良好的线性关系（r〉0．99）：在辣椒酱、面粉、醋和酱油4种样中，10种鼠药的加标回收率均在72．6％～112％范围内，相对标准偏差均不大于11．2％，检出限均在0．5～4．5μg／kg范围内。本方法快速、简便、灵敏、重现性好．能满足由此10种抗凝血类鼠药引发的突发性公共卫生安全事件的快述筛查与检测要求。A rapid method for the simultaneous screening and detection of ten anticoagulant rodenticides in foods was developed by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. After the extraction by acetonitrile and clean-up by QuEChERS, the extract was separated on a Poroshell 120 EC-Cl8 column （ 100 mm ×2. I mm, 2.7 μm） with the gradient elution of 5 mmol/L ammonium acetate and acetonitrile. The detec- tion was carried out by UPLC-MS/MS using a negative electrospray ionization interface in multi- ple reaction monitoring （MRM） mode. The ten anticoagulant rodenticides showed a good linear relationship （ r 〉 0.99） in the range of 5 - 500 μg/L . In the four samples of chili sauce, flour, vinegar and soy sauce, the spiked recoveries were in the range of 72.6% - 112%, and the rela- tive standard deviations （RSD） were all not more than I 1.2%. The limits of detection （LOD） were all in the range of 0.5 -4. 5 Iμg/kg. This method is rapid, simple, sensitive, accurate and of good specificity for the satisfactory rapid screening and detection of the ten anticoagulant rodenticides in the sudden public health security events.

关 键 词：超高效液相色谱-串联质谱 抗凝血类鼠药 食品 

分 类 号：O658[理学—分析化学]