超高效液相色谱-串联质谱法检测代用茶中的去甲乌药碱和曲托喹酚  

Determination of Higenamine and Tretoquinol in Substitute Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孟春杨 武茂瑞 吕绍芳 杨绍群 钟雪 毕珊[1] MENG Chunyang;WU Maorui;LYU Shaofang;YANG Shaoqun;ZHONG Xue;BI Shan(Guizhou Provincial Center for Disease Control and Prevention,Guiyang 550004,China;Guizhou Medical University,Guiyang 550000,China)

机构地区：[1]贵州省疾病预防控制中心,贵州贵阳550004 [2]贵州医科大学,贵州贵阳550000

出　　处：《食品科技》2025年第1期317-321,共5页Food Science and Technology

基　　金：贵州省卫生健康委科学技术基金项目(gzwkj2024-225,gzwkj2024-492);贵州省青年科学基金项目(2023-E-11)。

摘　　要：目的:建立超高效液相色谱串联质谱检测代用茶中去甲乌药碱和曲托喹酚的方法,并对42份代用茶中的去甲乌药碱和曲托喹酚含量进行检测。方法:称样后加入混合同位素内标,经混合溶剂(V_(甲醇):V_(水)=60:40)提取,离心后取上清液1 mL,加水1:1稀释混匀后上机。以0.1%甲酸水和甲醇为流动相梯度洗脱,用Agilent EclipsePlus C_(18)RRHD色谱柱分离,ESI^(+)模式进行多反应监测,内标法定量。结果:去甲乌药碱和曲托喹酚的线性范围为0.1~50.0μg/L,相关系数r均大于0.999,检出限(Limit of detection,LOD)为0.5μg/kg,定量限(Limit of quantification,LOQ)为1.5μg/kg。3个加标水平下(2、20、400μg/kg)去甲乌药碱的回收率为89.00%~108.07%,相对标准偏差(Relative standard deviation,RSD)为0.50%~8.02%;曲托喹酚的回收率为89.40%~108.77%,RSD在0.50%~3.73%。结论:该方法快速准确,适合代用茶中去甲乌药碱和曲托喹酚的批量检测。对42份代用茶进行检测,有7份样品检出去甲乌药碱,最高检出含量为4127.95μg/kg,为灵芝百合酸枣仁茶;未检出曲托喹酚。Objective:In order to establish a method for detecting higenamine and tretoquinol in substitute tea using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS)and to determine the contents of higenamine and tretoquinol in 42 substitute tea samples.Methods:After weighing the sample,a mixed isotope internal standard was added,followed by extraction using a mixed solvent(methanol:water=60:40,V/V).The supernatant(1 mL)was centrifuged,diluted with water(1:1),mixed,and analyzed by UPLC-MS.Separation was achieved using an Agilent EclipsePlus C_(18)RRHD column with a gradient elution of 0.1%formic acid water and methanol as the mobile phase.Detection was performed using positive electrospray ionization(ESI^(+))with multiple reaction monitoring,and quantification was achieved using the internal standard method.Results:The linear range for higenamine and tretoquinol was 0.1–50.0μg/L,with correlation coefficients(r)greater than 0.999.The limits of detection(LOD)and quantification(LOQ)were 0.5μg/kg and 1.5μg/kg,respectively.At three spiked levels(2,20,400μg/kg),the recovery rates for higenamine ranged from 89.00%to 108.07%,with relative standard deviations(RSDs)of 0.50%–8.02%.For tretoquinol,the recovery rates ranged from 89.40%to 108.77%,with RSDs of 0.50%–3.73%.Conclusion:The method is rapid and accurate,making it suitable for the batch determination of higenamine and tretoquinol in substitute tea.Among 42 substitute tea samples tested,7 samples were found to contain higenamine,with the highest detected content of 4127.95μg/kg,identified in Ganoderma lucidum,lily,and sour jujube kernel tea.Tretoquinol was not detected in any of the samples.

关 键 词：超高效液相色谱串联质谱 去甲乌药碱 曲托喹酚 代用茶 

分 类 号：TS207.5[轻工技术与工程—食品科学]