液相色谱-串联质谱法测定饲料中14种霉菌毒素及其类似物  

Simultaneous Determination of 14 Mycotoxins and Analogues in Feeds by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：应永飞[1] 朱聪英[1] 韦敏珏[1] 陈慧华[1] 屈健[1] 陆春波[1] 林仙军[1] 罗成江[1] 

机构地区：[1]浙江省畜产品质量安全检测中心,杭州310020

出　　处：《分析化学》2010年第12期1759-1764,共6页Chinese Journal of Analytical Chemistry

摘　　要：采用高效液相色谱-电喷雾串联质谱仪(LC-ESI-MS-MS),在多反应监测(MRM)模式下建立了饲料中玉米赤霉烯酮、黄曲霉毒素和单端孢霉烯族A类毒素等14种毒素及其类似物的快速确认测定方法。试样中的黄曲霉毒素、玉米赤霉烯酮和单端孢霉烯族A类毒素经乙腈-水(84:16,V/V)提取,正己烷脱脂及霉菌毒素多功能净化柱净化,氮气吹干,用1mL乙腈/水(1:1,V/V)定容后,进行液相色谱-串联质谱法测定,采用色谱保留时间和质谱碎片离子丰度比定性,外标法定量。采用正离子扫描和负离子扫描的方式进行仪器方法学研究,确定丰度比最高的2对离子作为监测离子,进行MRM模式定性定量分析。本方法的检出限(LOD)为0.1～0.8μg/kg;线性范围为2.0～200.0μg/L,相关系数r均大于0.999。在5.0～100μg/kg的添加水平上,上述14种霉菌毒素及其类似物的平均回收率为59.0%～107%;相对标准偏差为2.1%～12.6%。A liquid chromatography-mass spectrometric(LC-ESI-MS/MS) method for the determination of 14 mycotoxins and analogues(aflatoxin(AFB1),AFB2,AFM1,AFM2,AFG1,AFG2,α-zearanol(α-ZAL),β-ZAL,α-ZEL,β-ZEL,zearelone(ZAN),zearalenone(ZEN),toxin(HT-2),toxin(T-2) in feeds is reported.The drugs were extracted with acetonitrile/water(84:16,V/V) from analyte,then the solutions was purified by hexane liquid-liquid extraction and passing through multi-function cartridges.The eluent was evaporated by nitrogen blow,dissolved in acetonitrile/water(1:1,V/V) and then assayed by LC-MS/MS.The limits of detection(LOD) were 0.1-0.8 μg/kg.For these drugs,the calibration curves were linear between 2.0 to 200.0 μg/L,and the correlation coefficient was more than 0.999.The recoveries were 59.0%-107%,and the inter-relative standard deviation(n = 5) was 2.1%-12.6%,at spiked levels of 5.0-100 μg/kg.

关 键 词：高效液相色谱 串联质谱法 测定 饲料 霉菌毒素 其类似物 Mass Spectrometry 玉米赤霉烯酮 碎片离子 黄曲霉毒素 单端孢霉烯 相对标准偏差 色谱保留时间 类毒素 丰度比 方法学研究 定性定量分析 平均回收率 多反应监测 串联质谱仪 

分 类 号：S816.17[农业科学—饲料科学]