固相萃取-UPLC-MS/MS测定食品中的黄曲霉毒素M1和B1  

Determination of aflatoxin M1 and B1 in food by ultra- high performance liquid chromatography tandem mass spectrometry and solid phase extraction

作　　者：肖丽恒 何学梅 李萍 谢启明[2] 

机构地区：[1]楚雄州质量技术监督综合检测中心,云南楚雄675000 [2]楚雄师范学院化学与生命科学系,云南楚雄675000

出　　处：《楚雄师范学院学报》2013年第9期49-52,共4页Journal of Chuxiong Normal University

摘　　要：建立固相萃取与UPLC—MS／MS检测食品中黄曲霉毒素M1和黄曲霉毒素B1的方法。样品经乙腈提取和SPE小柱萃取净化，提取液经氮气吹干后，用50％甲醇水溶液定容。超高效液相色谱一串联质谱（UPLC—MS／MS）测定，采用电喷雾正离子（ESI＋）模式电离，多反应监测（MRM）模式检测。流动相为0．1％甲酸水溶液和甲醇，流速0．4ml／min，使用ZORBAX Eclipse XDB—C18色谱柱（100mm×3．0mm×1．8μm）为分析柱。黄曲霉毒素AFM1在0．1～50μg／kg范围内线性关系良好、黄曲霉毒素AFB1在0．1～10ug／kg范围内线性关系良好，相关系数均大于0．999；回收率在83．75％～97．8％之间；检出限AFMl为0．05μg／kg、AFBl0．02μg／kg。该法具有分析速度快，检测准确、灵敏度和回收率高等优点，适合食品中黄曲霉毒素M1、B1含量的检测。The method for detecting aflatoxin M1 （AFM1） and aflatoxin B1 （AFB1） from foods by solid -phase extraction and UPLC - MS/MS is established. The samples are extracted with acetonitrile and purified SPE column, then dried under nitrogen, and finally constant volume with 50% methanol water solu- tion. Ultra performance liquid chromatography -tandem mass spectrometry （UPLC -MS/MS） determination is experimented by the mode of electrospray positive ionization （ESI ＋ ） and multiple reaction monitoring （MRM）, and take methanol and 0.1% （v/v） formic acid aqueous solution as mobile phase, the flow rate is 0.4 ml/min, take ZORBAX Eclipse XDB - C18 chromatographic column （ 100 mm× 3.0 mm× 1.8 μm） as analytical column. AFM1 has a good linear relationship in the range of 0.1 - 50ug/kg and 0.1 - 10ug/kg for AFB1. The correlation coefficient are above 0. 999 both, and the recovery rate is 83.75% - 97.8%. The detection limit is 0.05 μg/kg for AFM1, 0.02 μg/kg for AFB1. The analytical method is fast, accurate detec- tion, sensitivity and recovery advantages, suitable for food aflatoxin M1 and B1 detection.

关 键 词：UPLC MS 黄曲霉毒素 食品 固相萃取 

分 类 号：R155.5[医药卫生—营养与食品卫生学]