超高效液相色谱-串联质谱法测定调味品中去甲乌药碱和曲托喹酚Determination of Higenamine and Tretoquinol in Condiments by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
王建凤,冯月超,周欣燃,张怡,楚弘宇,王颖,杨志超,刘艳
摘要(Abstract):
建立了超高效液相色谱-串联质谱法测定调味品中去甲乌药碱和曲托喹酚的分析方法,并对市售的44种调味品中去甲乌药碱和曲托喹酚的含量进行了调研。样品用含5%甲酸的乙醇溶液提取,经C_(18)、GCB以及EMR填料净化后,运用ACQUITY UPLC HSS T3色谱柱分离,电喷雾电离源正离子模式电离,多反应监测模式检测,内标法定量。结果表明,去甲乌药碱、曲托喹酚在0.05~5.00 ng/mL质量浓度范围内线性关系良好,相关系数(R)均大于0.995,去甲乌药碱在辣椒、辣酱、火锅底料、八角基质中的检出限和定量限分别为0.10,0.50μg/kg,在花椒和胡椒基质中的检出限和定量限分别为5.0,25.0μg/kg,而曲托喹酚的检出限和定量限在6类基质中一致,分别为0.03,0.10μg/kg,两种物质的平均回收率介于83.7%~118%之间,相对标准偏差小于16%,所调研的市售调味品中,均未检出曲托喹酚,70.4%样品中检出去甲乌药碱,含量介于0.56~1 962μg/kg之间。
关键词(KeyWords): 超高效液相色谱-串联质谱法;调味品;去甲乌药碱;曲托喹酚;食源性兴奋剂
基金项目(Foundation): 北京市改革与发展专项(2021ZL0115,23CB033)
作者(Author): 王建凤,冯月超,周欣燃,张怡,楚弘宇,王颖,杨志超,刘艳
参考文献(References):
- [1]WEI X H,ZHANG B P,LIANG X,et al.Higenamine alleviates allergic rhinitis by activating AKT1 and suppressing the EGFR/JAK2/c-JUN signaling[J].Phytomedicine,2021,86:153565-153578.
- [2]ZHU J X,LING W,XUE C,et al.Higenamine attenuates cardiac fibroblast abstract and fibrosis via inhibition of TGF-β1/Smad signaling[J].European Journal of Pharmacology,2021,900:174013-174022.
- [3]DENG T,WEI Z M,GAEL A,et al.Higenamine improves cardiac and renal fibrosis in rats with cardiorenal syndrome via ASK1 signaling pathway[J].Journal of Cardiovascular Pharmacology,2020,75(6):535-544.
- [4]WEN J X,LI M J,ZHANG W W,et al.Role of higenamine in heart diseases:a mini-review[J].Frontiers in Pharmacology,2022,12:798495-798507.
- [5]杨明,何思睿,张丹,等.常用药材中去甲乌药碱的LC-MS/MS测定方法研究[J].中国测试,2018,44(3):61-65.
- [6]张正,陈宝玲,郑英丽,等.3H-去甲乌药碱的合成[J].中华核医学杂志,2003(3):49-50.
- [7]田海峰.柱前衍生化反相高效液相色谱法分析去甲乌药碱[D].延吉:延边大学,2011.
- [8]WANG R,XIONG X P,YANG M,et al.A pharmacokinetics study of orally administered higenamine in rats using LC-MS/MS for doping control analysis[J].Drug Test Analysis,2020,12(4):485-495.
- [9]KOZHUHAROV V R,IVANOV K,IVANOVA S.Higenamine in plants as a source of unintentional doping[J].Plants,2022,11:354-370.
- [10]YEN C C,TUNG C W,CHANG C W,et al.Potential risk of higenamine misuse in sports:evaluation of lotus plumule extract products and a human study[J].Nutrients,2020,12:285-301.
- [11]OKANO M,SATO M,KAGEYAMA S.Determination of higenamine and coclaurine levels in human urine after the administration of a throat lozenge containing Nandina domestica fruit[J].Drug Test Analysis,2017,9(11-12):1788-1793.
- [12]杨明,陈丹,涂凤琴,等.高效液相色谱-串联质谱测定香辛料中的去甲乌药碱[J].现代食品科技,2020,36(3):275-280.
- [13]FENG Y R,WANG B,LI G J,et al.Determination of higenamine in multi-matrix by gas chromatography-mass spectrometry combined with derivatization technology[J].Journal of Food and Drug Analysis,2020,28(1):124-131.
- [14]YAN K,WANG X,WANG Z,et al.The risk of higenamine adverse analytical findings following oral administration of plumula nelumbinis capsules[J].Drug Test Analysis,2019,11(11-12):1731-1736.
- [15]YANG M,CHEN D,TU F Q,et al.Determination of higenamine in spices by high performance liquid chromatography-tandem mass spectrometry[J].Modern Food Science and Technology,2020,36:1-7.
- [16]ZHANG N N,LIAN Z Q,PENG X Y,et al.Applications of higenamine in pharmacology and medicine[J].Journal of Ethnopharmacology,2021,13(10):1776-1782.
- [17]王晗,汤一铸,赵晓亚,等.QuEChERS与液相色谱-串联质谱联用检测中药、调味品及外敷药物中去甲乌药碱的含量[J].色谱,2019,37(10):1036-1041.
- [18]GRUCZA K,KWIATKOWSKA D,KOWALCZYK K,et al.Analysis for higenamine in urine by means of ultra-high-performance liquid chromatography-tandem mass spectrometry:interpretation of results[J].Drug Test Analysis,2018,10(6):1017-1024.
- [19]CHANG W C W,YEN C C,LIU W Y,et al.Blood-to-muscle distribution and urinary excretion of higenamine in rats[J].Drug Test Analysis,2021,13(10):1776-1782.
- [20]FENG S,HU P,JIANG J.Determination of higenamine in human plasma and urine using liquid chromatography coupled to positive electrospray ionization tandem mass spectrometry[J].Journal of Chromatography B,2011,879(11-12):763-768.
- [21]ZHAO X X,YUAN Y L,WEI H,et al.Identification and characterization of higenamine metabolites in human urine by quadrupole-orbitrap LC-MS/MS for doping control[J].Journal of Pharmaceutical and Biomedical Analysis,2022,214:114732-114742.
- [22]STAJIC A, ANDELKOVI C M, DIKI C N,et al.Determination of higenamine in dietary supplements by UHPLC/MS/MS method[J].Journal of Pharmaceutical and Biomedical Analysis,2017,30(146):48-52.
- [23]李燕,贺亚男,黄浩洲,等.液质联用技术追踪生物碱类成分在川乌茎叶生长周期的动态变化规律[J].中草药,2019,50(8):1985-1991.
- [24]YAN Y H,LIAN K Q,LYU P,et al.Determination of higenamine and tretoquinol in spices by solid phase extraction-isotope internal standard-high performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Composition and Analysis,2022,110:104524-104531.
- [25]张寒霜,赵发,韩晓晓,等.超声辅助提取-氢化物原子荧光光谱法测定香辛料中的铅[J].中国调味品,2022,47(3):176-179.
- [26]蒋孟圆,陈俊秀,农蕊瑜,等.市售调味酱中5种真菌毒素的测定[J].中国调味品,2022,47(3):160-163.
- [27]阳凤娇,李珍艳,吴雪琪,等.QuEChERS-HPLC测定郫县豆瓣酱中真菌毒素污染的研究[J].中国调味品,2023,48(1):181-186.
- [28]张哲,张莹,赵桐,等.超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量[J].中国调味品,2023,48(1):181-186.
- [29]蒋莹,邢政,吴婷,等.卤汤中5种香辛料主效成分的提取检测和溶出规律研究[J].中国调味品,2022,47(9):1-6,14.
- [30]NUNTAWONG P,OCHI A,CHAINGAM J,et al.The colloidal gold nanoparticle-based lateral flow immunoassay for fast and simple detection of plant-derived doping agent,higenamine[J].Drug Test Analysis,2021,13(4):762-769.
- [31]冯月超,王建凤,侯帆,等.QuEChERS结合超高效液相色谱-串联质谱法同时测定畜禽肉中44种食源性兴奋剂和6种孕激素[J].色谱,2022,40(5):409-422.
- [32]XU Z Y,XIAO X,JIANG X B,et al.Methodology for analysing pesticide multi-residue in Wuyi rock tea using modified QuEChERS followed by gas chromatography-tandem mass spectrometry[J].Applied Ecology and Environmental Research,2021,19(2):1517-1533.
- [33]LUO P,LIU X H,KONG F,et al.Simultaneous determination of 169 veterinary drugs in chicken eggs with EMR-lipid clean-up using ultra-high performance liquid chromatography tandem mass spectrometry[J].Analytical Methods,2019,12:1657-1662.