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

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0.25~50μg/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0.05μg/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.

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. 25~50μg/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.