基于Q-Exactive高分辨质谱的蒙中药材苦参化学成分的快速分析鉴定
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摘要
目的:运用高效液相色谱串联四极杆-静电场轨道阱高分辨质谱(HPLC-Q-ExactiveMS)建立一种对苦参复杂成分实现精准、高效、快速分析鉴定的方法。方法:采用Agilent Zorbax SB-Aq色谱柱(150 mm×4.6 mm,5μm),以5 mmol/L乙酸铵/0.1%甲酸水溶液(A)-乙腈(B)为流动相梯度洗脱,采用热电喷雾(HESI)质谱离子源,在正、负离子模式下采集数据,依据精确质量数和Chemspider数据库确定化合物分子式及结构式,通过比较对照品及文献报道的保留时间、一级质谱以及二级碎片离子,结合此类化合物的裂解规律,对其进行准确结构鉴定。结果:共鉴定了49个化合物,其中12个异戊二烯黄酮类和3个生物碱类化合物为该药材首次鉴定。结论:该方法可系统、准确、快速鉴定苦参复杂化学成分,为阐明该药材的物质基础以及制定质量标准提供了实验依据。
引文
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[2] Liu Y,Mo ZX,Wang CG,et al.Identification of metabolites of kurarinone from Sophora flavescens Ait.in rat urine by ultra-performance liquid chromatography with linear ion trap orbitrap mass spectrometry[J].Tropical Journal of Pharmaceutical Research,2016,15(6):1299-1305.
[3] 赵琴琴,张玉峰,范骁辉.高效液相色谱多级质谱联用法同时鉴定苦参中的两大类活性成分[J].中国中药杂志,2011,36(6):762-769.
[4] Liu G,Dong J,Wang H,et al.Characterization of alkaloids in Sophora flavescens Ait.by high-performance liquid chromatography-electrospray ionization tandem mass spectrometry[J].Journal of Pharmaceutical & Biomedical Analysis,2011,54(5):1065-1072.
[5] Weng Z,Zeng F,Zhu Z,et al.Comparative analysis of sixteen flavonoids from different parts of Sophora flavescens Ait.by ultra high-performance liquid chromatography-tandem mass spectrometry[J].J Pharm Biomed Anal,2018,156:214-220.
[6] Zhang Y,Zhang P,Cheng Y.Structural characterization of isoprenylated flavonoids from Kushen by electrospray ionization multistage tandem mass spectrometry.[J].Journal of Mass Spectrometry,2008,43(10):1421-1431.
[7] Liu Y,Chen L,Cai W,et al.Use of an UHPLC-MS/MS method for determination of kuraridin and characterization of its metabolites in rat plasma after oral administration[J].Molecules,2018,23(2):132.
[8] 孙国东,霍金海,程团,等.基于UPLC-Q-TOF/MS技术的胡桃楸叶化学成分分析[J].中药材,2017,40(5):1123-1129.
[9] Fan RX,Liu R,Ma R,et al.Determination of oxymatrine and its active metabolite matrine in human plasma after administration of oxymatrine oral solution by high-performance liquid chromatography coupled with mass spectrometry[J].Fitoterapia,2013,89(1):271-277.
[10] 王长生,董红娇,包雅婷,等.UPLC-Q-Exactive四级杆-静电场轨道阱高分辨质谱联用快速分析粗茎秦艽化学成分[J].中草药,2016,47(18):3175-3180.