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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
【摘要】 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 m in和8.8m in,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/z352、528和m/z336、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。
【Abstract】 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 mL/min 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 electrospray-(positive) 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.
【Key words】 Liquid chromatography-electrospray ionization tandem mass spectrometry; fumonisin; asparagus; corn;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2005年11期
- 【分类号】TS207.3
- 【被引频次】44
- 【下载频次】515