超高压高效液相色谱——电喷雾串联质谱法测定花粉中的12种生物毒素  

High Performance Liquid Chromatography——Electrospray Tandem Mass Spectrometry Method for the Determination of 12 Kinds of Biological Toxins in Pollen

作　　者：王飞[1] 刘晓茂[1] 张鸿雁 李学民[1] 张静[1] 

机构地区：[1]秦皇岛出入境检验检疫局,河北秦皇岛066004 [2]黑河出入境检验检疫局,黑龙江黑河164300

出　　处：《黑河学院学报》2013年第4期121-125,共5页Journal of Heihe University

基　　金：河北出入境检验检疫局科技计划项目<蜂产品中多种真菌毒素检测方法的研究与应用>(HE2011K018)

摘　　要：用正己烷饱和的乙腈溶液提取花粉中12种生物毒素，加入乙腈饱和-正己烷溶液去除色素和油脂干扰，旋蒸后用乙腈-水溶液（4＋1）溶解固相萃取柱净化分离，UPLC／ESI—MS进行检测。在线性关系内，r〉0．9991，黄曲霉毒素B1、B2、G1、G2定量限（LOQ）为0．5μg/kg，赭曲霉毒素、伏马毒素B。定量限（LOQ）为100μg/kg，玉米赤霉烯酮、a-玉米赤霉醇、B-玉米赤霉醇、B-玉米赤霉烯醇、a-玉米赤霉烯醇、玉米赤霉酮的定量限（LOQ）均为0．5μg/g，回收率77．0％-127％。重复性相对标准偏差（RsDr）小于9．9％，再现性相对标准偏差（RSDR）小于16．9％。方法有良好的精密度和重现性，适用于花粉的检测。Extraction of 12 kinds of biological toxins in pollen n -hexane saturated with acetonitrile solu- tion, adding acetonitrile saturated solution in hexane to remove pigment and lipid. Using acetonitrile and water （4 ＋ 1 ） dissolved solid phase extraction column purification separation after rotary evaporation. Detection was performed by UPLC/ESI- MS,which is greater than 0.9991 in Online relationships. The quantitation limit of atlatoxins B1 ,aflatoxins B2 ,aflatoxins G1 ,aflatoxins G2 were 0.5μg/kg,and the quantitation limit of Ochratoxin A, ,fumonisin B1 were 100 μg/kg. The quantitation limit of Zearalenone, ct - Zeranol, α - Zeranol, β- Zearalenol enol, α-Zearalend enol, Zearalanone were 0.5 μg/kg. The average recovery is 77.0% - 127 %. Repeatability relative standard deviation is less than 9.9% , reproducibility relative standard deviation （ RS- DR） of less than 16.9%. The method is suitable for detection of pollen and has good precision and reproducibility.

关 键 词：花粉 生物素 超高压液相质谱 

分 类 号：O558[理学—热学与物质分子运动论]