固相萃取-高效液相色谱-串联质谱法检测粮食及其制品中的呕吐毒素  

Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry

作　　者：黄娟[1] 陈国松[2] 张晓燕[1] 沈崇钰[1] 吕辰[2] 吴斌[1] 刘艳[1] 陈惠兰[1] 丁涛[1] 

机构地区：[1]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001 [2]南京工业大学理学院,江苏南京210009

出　　处：《色谱》2012年第11期1203-1207,共5页Chinese Journal of Chromatography

基　　金：江苏检验检疫局科研项目(2010KJ32)

摘　　要：建立了粮食及其制品中呕吐毒素的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈-水(84∶16,v/v)溶液提取,HLB固相萃取柱富集净化,采用HPLC-MS/MS法对目标物进行定性确证和定量分析。在Phe-nomenex Kinetex C18柱(100 mm×4.6 mm,2.6μm)上以0.3‰氨水和乙腈为流动相进行梯度洗脱分离;质谱模式为电喷雾负离子监测模式。本方法的检出限(以信噪比(S/N)=3计)和定量限(以S/N=10计)分别为20μg/kg和50μg/kg;在20～1 000μg/L范围内呈现良好的线性关系,相关系数(r)大于0.99。对本底空白的面粉、大麦、大豆、大米、玉米粉、木薯干、小麦等7种代表性基质进行50、100、500μg/kg 3个含量水平的添加试验,回收率范围为75.6%～111.0%,精密度(以相对标准偏差(RSD)计)不大于13.0%。本方法准确可靠,灵敏度高,经济实用,可替代较为昂贵的免疫亲和柱和多功能净化柱,较大地降低检测成本。A method was established for the determination of deoxynivalenol（vomitoxin） in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The sample was firstly extracted by acetonitrile-water（84∶16,v/v）.The extract was then cleaned-up by an HLB solid phase extraction cartridge.The separation was carried out on a Phenomenex Kinetex C18 column（100 mm×4.6 mm,2.6μm） with a gradient elution using 0.3‰ ammonia solution-acetonitrile as mobile phases.The analysis of deoxynivalenol was performed under electrospray negative ionization mode.The limit of detection（LOD,S/N=3） and the limit of quantification（LOQ,S/N=10） were 20 μg/kg and 50 μg/kg,respectively.A good linearity（r0.99） was achieved for the target compound over the range of 20-1 000 μg/L.The recoveries at the three spiked levels（50,100,500 μg/kg） in the blank matrices such as flour,barley,soybean,rice,cornmeal,cassava and wheat,were varied from 75.6% to 111.0% with the relative standard deviations no more than 13.0%.The method is accurate,efficient,sensitive and practical.The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

关 键 词：固相萃取 高效液相色谱-串联质谱 呕吐毒素 粮食 粮食制品 

分 类 号：O658[理学—分析化学]