液相色谱-电喷雾串联质谱法测定食品中的伏马菌素

Determination of Fumonisin in Food by High Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

通过固相萃取富集伏马菌素,采用液相色谱-电喷雾串联质谱法测定玉米和芦笋中的伏马菌素B1(FB1)、伏马菌素B2(FB2).在最佳色谱条件下,伏马菌素B1、伏马菌素B2的保留时间分别为5.2 min 和8.8 min,样品空白无干扰.离子化技术采用电喷雾正离子方式,以多反应监测(MRM)方式进行检测.该法检出限为80 pg;线性定量范围为0.01～10mg/L;回收率为78.3%～104.9%;相对标准偏差为2.2%～14.2%.利用ESI/MS/MS对伏马菌素B1、伏马菌素B2进行了质谱解析,分别选择特征离子峰m/z 352、528和m/z 336、512作为伏马菌素B1、伏马菌素B2准确定性的依据.方法灵敏度高,选择性好,准确度高,可为食品中伏马菌素的风险评估提供灵敏、准确的分析方法.

High performance liquid chromatography-electrospray ionization tandem mass spectrometry （ESI/MS/MS） combining with solid phase extraction has been developed for the determination of fumonisin B1 （FB1 ） and fumonisin B2 （FB2 ） in corn and asparagus. The gradient program was used to obtain an optimal separation with mobile phase of MeOH：H2O：trifluoroacetic acid at 0. 8 mlMmin on a C8 column. The retention time of FB1 and FB2 were 5.2 min and 8.8 min, respectively. Ionization was performed in an electrospraypositive ion source （ ＋ ） and quantitative detection was carried out using Multiple Reaction Monitor mode. The limit of detection was 80 pg and the linear range was from 0. 01 to 10 mg/L with recovery of 78.3% - 104. 9% and the RSD from 2.2 to 14.2%. Using the proposed ESI/MS/MS, FB1 and FB2 could be identified with both retention time and the typical ion peaks for FB1 at m/z 532 and 528 and FB2 at m/z 336, 512, respectively. The method was proved to be validated to analyze these two fumonisins from asparagus and corn samples.