基质分散固相萃取-超高效液相色谱串联质谱法同时测定茶叶中17种卡西酮类物质  

Simultaneous determination of 17 cathinones compounds in tea by matrix dispersed solid phase extraction-ultra high performance liquid chromatographytandem mass spectrometry

作　　者：王巧霞 孙润之 叶洪 唐庆强 傅红[1] 陈燕雯 杨方 WANG Qiaoxia;SUN Runzhi;YE Hong;TANG Qingqiang;FU Hong;CHEN Yanwen;YANG Fang(College of Biological Science and Engineering,Fuzhou University,Fuzhou 350108,China;Technology Center of Fuzhou Customs,Fuzhou 350001,China;Fuzhou International Travel Healthcare Centre,Fuzhou 350001,China;College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350002,China;Comprehensive Technology Service Center of Sanming Customs,Sanming 365001,China)

机构地区：[1]福州大学生物科学与工程学院,福州350108 [2]福州海关技术中心,福州350001 [3]福州国际旅行卫生保健中心,福州350001 [4]福建农林大学食品科学学院,福州350002 [5]三明海关综合技术服务中心,三明365001

出　　处：《分析试验室》2024年第11期1620-1625,共6页Chinese Journal of Analysis Laboratory

基　　金：福建省自然基金项目(2020J1098);福建省科技计划项目(2021I0033);海关总署科研项目(2020HK188;2021HK197);福州市科技计划项目(2020-S-34)资助。

摘　　要：建立了同时测定茶叶中17种卡西酮类物质的超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)方法。样品以乙腈提取,150 mg N-丙基乙二胺(PSA)和100 mg石墨化炭墨(GCB)分散固相萃取净化,乙腈和20 mmol/L乙酸铵-0.1%甲酸溶液为流动相,五氟苯基色谱柱(2.1 mm×100 mm,5μm)分离,正离子模式电喷雾电离,多反应监测模式(MRM)测定,基质匹配标准工作曲线外标法定量。结果表明,7 min内可完成17种卡西酮类物质的检测,方法在0~100μg/L范围内具有良好的线性关系,相关系数均大于0.996。方法的检出限和定量限分别为0.2~0.5μg/kg和1~2μg/kg。在空白样品中进行2,4,20μg/kg加标回收实验,17种卡西酮类物质的回收率为70.9%~117.4%,相对标准偏差为0.7%~11%。An ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry method was established for the simultaneous determination of 17 cathinones compounds in tea.The cathinones in tea sample were firstly extracted by acetonitrile,and the extracts were purified by solid-phase disperse with 150 mg PSA and 100 mg GCB,and the separation was completed on a pentafluorophenyl column (2.1 mm×100 mm,5μm) with a gradient system of mixture of acetonitrile and 20 mmol/L ammonium acetate containing 0.1%formic acid solution as mobile phase.Multi-reaction monitoring (MRM) was employed for mass spectrometry determination with matrix calibration curve external standard method for quantification.The 17 cathinones can be detected within 7 min.The linear ranges of 17 cathinones were 0-100μg/L,the limits of detection and quantification were 0.2-0.5μg/kg and 1-2μg/kg,respectively.The correlation coefficients were higher than 0.996.The recoveries of 17 cathinones were 70.9%-117.4%at three spiked levels of 2,4,20μg/kg,and relative standard deviations were 0.7%-11%.

关 键 词：茶叶 超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS) 卡西酮类物质 分散固相萃取 

分 类 号：TS207.3[轻工技术与工程—食品科学]