中国中药杂志

2021, v.46(17) 4456-4461

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UPLC-MS/MS测定一点红不同部位中6种吡咯里西啶生物碱的含量
Simultaneous determination of six pyrrolizidine alkaloids in different parts of Emilia sonchifolia by UPLC-MS/MS

昝珂;周颖;李耀磊;王莹;刘丽娜;金红宇;左甜甜;马双成;
ZAN Ke;ZHOU Ying;LI Yao-lei;WANG Ying;LIU Li-na;JIN Hong-yu;ZUO Tian-tian;MA Shuang-cheng;National Institutes for Food and Drug Control;NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine), Zhejiang Institute for Food and Drug Control;

摘要(Abstract):

建立同步测定一点红不同部位中N-氧化印美定(ImNO)、N-氧化石松胺(LyNO)、千里光菲灵碱(Sp)、N-氧化千里光菲灵碱(SpNO)、N-氧化千里光宁碱(SnNO)和克氏千里光碱(Sk)等6种吡咯里西啶生物碱的UPLC-MS/MS方法。采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8μm),以含0.05%甲酸和2.5 mmol·L~(-1)甲酸铵的水溶液(A)及含0.05%甲酸和2.5 mmol·L~(-1)甲酸铵的乙腈溶液(B)为流动相,梯度洗脱;电喷雾离子源,正离子多反应模式监测,外标法测定。定量结果显示,一点红的不同部位中吡咯里西啶生物碱有一定差异,Sk在4个部位均有检出,并且含量大致相等;SnNO也存在于各个部位中,但根中较其他部位明显偏高;Sp和SpNO存在于根和花中,且根中含量高于花中;ImNO和LyNO仅存在叶中,含量较低。所测的6种成分中ImNO、LyNO和SpNO均为首次从该药材中发现并进行了含量测定,丰富了该药材的毒性成分种类,为该药材的质量评价及安全用药提供科学依据。
This study aims to develop a UPLC-MS/MS method for simultaneous determination of six pyrrolizidine alkaloids(PAs)--intermedine N-oxide(ImNO), lycopsamine N-oxide(LyNO), seneciphylline(Sp), seneciphylline N-oxide(SpNO), senecionine N-oxide(SnNO), and senkirkine(Sk) in different parts of Emilia sonchifolia. UPLC conditions are as follows: ACQUITY UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm), mobile phase consisting of 0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in water(A)-0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in acetonitrile(B) for gradient elution. MS conditions are as below: electrospray ionization(ESI) in the positive ion mode, multiple reaction monitoring(MRM), and the content of the six PAs was calculated with the external standard method. The results suggested the differences in the six PAs among different parts of E. sonchifolia. Sk was detected in all the four parts, with similar content. SnNO also existed in all the four parts, but the content in roots was significantly higher than that in other parts. Sp and SpNO were found in both roots and flowers, with the content higher in the former than in the later. ImNO and LyNO were only found in leaves, and the content was low. Among the six components detected, ImNO, LyNO, and SpNO were found and determined for the first time, which enriched the toxic components and laid a scientific basis for the quality and safety evaluation of E. sonchifolia.

关键词(KeyWords): 一点红;不同部位;吡咯里西啶生物碱;超高效液相色谱-串联质谱;含量测定
Emilia sonchifolia;different part;pyrrolizidine alkaloids;UPLC-MS/MS;content determination

Abstract:

Keywords:

基金项目(Foundation): 国家“重大新药创制”科技重大专项(2018ZX09303-024,2018ZX09735-006)

作者(Author): 昝珂;周颖;李耀磊;王莹;刘丽娜;金红宇;左甜甜;马双成;
ZAN Ke;ZHOU Ying;LI Yao-lei;WANG Ying;LIU Li-na;JIN Hong-yu;ZUO Tian-tian;MA Shuang-cheng;National Institutes for Food and Drug Control;NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine), Zhejiang Institute for Food and Drug Control;

Email:

DOI: 10.19540/j.cnki.cjcmm.20210623.202

参考文献(References):

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