在线固相萃取-液相色谱-串联质谱法快速测定玉米粉和面粉中伏马毒素  

On-Line Solid Phase Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry for Determination of Fumonisins in Corn and Wheat Flour Samples

作　　者：马俊美 刘东 张雷雷 沈璐 王丽霞 张岩 MA Junmei;LIU Dong;ZHANG Leilei;SHEN Lu;WANG Lixia;ZHANG Yan(Hebei Food Inspection and Research Institute, Shijiazhuang 050200, China;Hebei Food Safety Key Laboratory ,Shijiazhuang 050200, China)

机构地区：[1]河北省食品检验研究院,河北省食品安全重点实验室,河北石家庄050200

出　　处：《食品科学》2017年第20期300-305,共6页Food Science

基　　金：河北省食品药品监督管理局食品安全科技计划项目(PT2014028;PT2014033);“十二五”国家科技支撑计划项目(2015BAK36B03);国家重大科学仪器设备开发专项(2012YQ03011110)

摘　　要：建立在线固相萃取-液相色谱-串联质谱法检测玉米粉和面粉中3种伏马毒素的分析方法。样品用乙腈-水(50∶50,V/V)提取,提取液直接上样,经过WAX在线固相萃取柱净化,以0.1%甲酸溶液和乙腈为流动相,经XBridge C_(18)色谱柱分离,采用电喷雾正电离多反应模式监测,内标法定量。结果表明:伏马毒素B1、伏马毒素B2和伏马毒素B3在0.05~50 ng/m L之间线性关系良好,相关系数均大于0.999 0;检出限和定量限分别为0.08μg/kg和0.2μg/kg;添加水平为0.2~50.0μg/kg时,方法回收率范围为93.9%~117.8%,相对标准偏差范围在1.8%~9.4%。此方法简便快速、灵敏度高,可用于玉米粉和面粉中伏马毒素的准确定量。An analytical method was developed to determine three fumonisins in corn and wheat flour samples using online solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry(HPLCMS-MS).Samples were extracted with an acetonitrile-water mixture(50:50,V/V)and purified with an on-line solid phase extraction column(WAX column).The fumonisins were separated on an XBridge C18colum by using0.1%formic acid solution mixed with acetonitrile as the mobile phase.Multiple reaction monitoring was used to acquire mass spectrometric data under positive electrospray ionization mode.The internal standard method was adopted for quantification.The results showed that good linearity was obtained in the range of0.05-50ng/mL for fumonisin B1,fumonisin B2and fumonisin B3,and the correlation coefficients were all greater than0.9990.The limits of detection(LOD)and quantitation(LOQ)for these analytes were0.08and0.2μg/kg,respectively.Recoveries of the method were in the range of93.9%-117.8%at spiked levels between0.2and50μg/kg,and precision(expressed as relative standard deviation)ranged from1.8%to9.4%.The developed method could be used for the accurate quantitative measurement of fumonisins in corn and wheat flour samples.

关 键 词：在线固相萃取净化 液相色谱-串联质谱 同位素稀释 伏马毒素 

分 类 号：O657.63[理学—分析化学]