分析测试新方法(210~214)超高效液相色谱-串联质谱法测定花椒中罗丹明B的含量

Determination of Rhodamine B in Zanthoxylum Bungeanum Maxim by Ultra Performance Liquid Chromatography- Tandem Mass Spectrometry

  • 摘要: 建立了一套固相萃取结合超高效液相色谱-串联质谱法测定花椒中罗丹明B含量的分析方法. 样品经20%丙酮正己烷溶液提取后,采用中性氧化铝固相萃取柱进行净化处理. 以乙腈-0.1%甲酸水溶液作流动相,C18色谱柱分离,多重反应监测正离子扫描模式下进行检测. 罗丹明B在 0.25~50 μg/kg浓度范围内,线性方程为y=2800.6x-113.6,线性相关系数r=0.99993,方法检出限0.05 μg/kg,RSD为1.75%~2.29%,回收率在89%~102%之间. 方法操作简便,检出限低,结果准确可靠,可以用于花椒中罗丹明B的含量分析.

     

    Abstract: A method based on the ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) has be developed for the determination of rhodamine B in zanthoxylum bungeanum maxim.The sample was extracted with 20 % acetone-normal hexane and then cleaned up by the Cleanert Alumina-N-SPE. The target analytes were separated on a C18 column using acetonitrile and water containing 0.1% formic acid as the mobile phases, and were detected by a multiple reaction monitoring positive model.Under optimized detection conditions,the linear range for rhodamine B were 0.25~50 μg/kg.The linear equation was y=2800.6x-113.6,the coefficient of correlation was r=0.99993.The limits of quantification was 0.05 μg/kg. The relative standard deviations of reproducibility were 1.75%~2.29%. The recoveries of the method were 89%~102%. The method is simple, rapid, highly sensitive, and is suitable for the determination of rhodamine B in zanthoxylum bungeanum maxim.

     

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