液相色谱-串联质谱法测定饲料中黄曲霉毒素的研究  

Determination of Aflatoxins in Feeds by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：朱聪英[1] 应永飞[1] 韦敏珏[1] 陈慧华[1] 陆春波[1] 周文海[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,浙江杭州310020

出　　处：《质谱学报》2010年第4期240-246,共7页Journal of Chinese Mass Spectrometry Society

摘　　要：建立了液相色谱-串联质谱法测定饲料中6种黄曲霉毒素（包括黄曲霉毒素B1、B2、G1、G2、M1、M2）的方法。试样中的黄曲霉毒素经84％乙腈溶液超声提取后，用正己烷脱脂，过霉菌毒素多功能固相萃取柱净化，氮气吹至干，用流动相溶解后进行液相色谱-串联质谱法测定。方法的最低检出限为0．2μg·kg^-1，定量限均为0．5μg·kg^-1；标准工作液在0．5-100μg·L^-1的范围内线性良好；加标浓度在1．0-100μg·kg^-1范围内，饲料中黄曲霉毒素的回收率在66．1％～108％之间，批内相对标准偏差≤17．8％，能满足相关法规要求。Totally 6 Aflatoxins in feeds were determined by high performance liquid chroma- tography combined with electrospray ionization triple quadrupole tandem mass spectrometry （HPLC-MS/MS） under the multiple reaction monitoring （MRM） mode, and especially fo- cused on the optimization of extraction, clean-up, HPLC separation and MS/MS parameters of analytes. The Aflatoxins B1, B2, G1, G2, M1 and M2 were extracted by 84 % of acetoni- trile aqueous solution, purified by passing through multifunctional cartridges. The elution was evaporated by nitrogen blow and dissolved by mobile phase, and then assayed by HPLC-MS/MS. The limits of detection（LOD） are 0.2 μg · kg^-1 , and the limits of quanti- tation（LOQ） are 0.5 μg · kg^-1. The calibration curves are linear between 0.5 μg ·L-1 and 100 μg ·L ^-1 for Aflatoxins B1, B2, G1, G2, M1 and M2. Recoveries of those mycotoxins in feeds are 66.1%-108%, and inter-relative standard deviation（n=5） is less than 17.8% at spiked level of 1.0-100μg · kg-1. The method is simple, sensitive and reliable for feed safety.

关 键 词：液相色谱-串联质谱法(LC-MS/MS) 黄曲霉毒素 饲料 

分 类 号：O657.63[理学—分析化学]