猪胃组织中脱氧雪腐镰刀菌烯醇的液质联用检测  

Detection of deoxynivalenol in gastric tissue of pig by LC-MS/MS method

作　　者：卢培成[1] 剡海阔[1] 曾振灵[1] 贺利民[1] 梁梓森[1] 范小龙[1] 邓衔柏[1] 邹新华 

机构地区：[1]华南农业大学兽医学院,广东广州510642 [2]八维生物科技有限公司,江西赣州341200

出　　处：《广东农业科学》2011年第9期114-116,125,共4页Guangdong Agricultural Sciences

基　　金：国家"973"计划项目(C120201)

摘　　要：以脱氧雪腐镰刀菌烯醇毒素(Deoxynivalenol,DON)为检测对象,建立了一种检测猪胃组织中DON的液质联用分析方法。样品经乙腈:水(80:20,V/V)提取,varian Bond Elut Mycotoxin净化柱净化后,收集提取液并于45℃水浴氮气吹干,乙腈:水(20:80,V/V)溶解,经0.22μm微孔滤膜过滤后,以反相C18柱为色谱柱,甲醇、纯水溶液梯度洗脱为流动相,电离离子源电离后质谱检测。结果显示,DON在2～100 ng/mL范围内线性关系良好(r2>0.99);检测限(LOD)和定量限(LOQ)分别为2μg/g和5μg/g;低、中、高浓度(5、20、50μg/g)的回收率分别为71.8%、89.5%、87.4%,RSD分别为6.75%、9.82%、6.39%。表明该方法操作简单,灵敏度高,适用于猪胃组织中DON的检测。The appropriate method of liquid chromatography-mass spectrometry（LC-MS/MS）was built for detecting deoxynivalenol（DON） in gastric tissue of pig.The DON was extracted by the solution that acetonitrile∶H2O（80∶20,V/V） cleaned up by varian Bond Elut Mycotoxin clean-up column,evaporated to dryness at 45℃ water bath by nitrogen,dissolved by acetonitrile∶water（20∶80,V/V）solution and filtrated through 0.22 μm micromembrane.After that,the deoxynivalenol mycotoxin were separated in a Reversed-phase C18 chromatographic column with mobile phase of methanol and ultra-pure water and ionized by the chemical ionization.The signals of the mycotoxins were detected by mass spectrometry to qualification and quantization.The results showed that good linear correlations between the peak area and toxin concentration were found;the linear range for DON was 2～100 ng/mL（r20.99）;limit of detection（LOD）was 2 μg/mL and limit of quantitation（LOQ） was 5 μg/mL;the recoveries of low,medium and high concentration： 5 μg/g,20 μg/g and 50 μg/g were 71.8%,89.5% and 87.4%,respectively;RSD were 6.75%,9.82%,6.39%,respectively.The results indicated that this method was not only quantitatively accurate,but also high sensitive and convenient for operation,and suitable for detection of gastric tissue deoxynivalenol.of pig.

关 键 词：液相色谱-质谱联用 猪 胃组织 脱氧雪腐镰刀菌烯醇 

分 类 号：S852.6[农业科学—基础兽医学]