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采用超高效液相色谱-光电二极管阵列-质谱联用技术对蛇根木根中的生物碱进行定量和表征。

Quantification and characterization of alkaloids from roots of Rauwolfia serpentina using ultra-high performance liquid chromatography-photo diode array-mass spectrometry.

作者信息

Sagi Satyanarayanaraju, Avula Bharathi, Wang Yan-Hong, Khan Ikhlas A

机构信息

National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, 1558 University Circle, University, MS, 38677, USA.

Division of Pharmacognosy, Department of BioMolecular Sciences, School of Pharmacy, The University of Mississippi, University, MS, 38677, USA.

出版信息

Anal Bioanal Chem. 2016 Jan;408(1):177-90. doi: 10.1007/s00216-015-9093-4. Epub 2015 Oct 17.

Abstract

A new UHPLC-UV method has been developed for the simultaneous analysis of seven alkaloids [ajmaline (1), yohimbine (2), corynanthine (3), ajmalicine (4), serpentine (5), serpentinine (6), and reserpine (7)] from the root samples of Rauwolfia serpentina (L.) Benth. ex Kurz. The chromatographic separation was achieved using a reversed phase C18 column with a mobile phase of water and acetonitrile, both containing 0.05% formic acid. The seven compounds were completely separated within 8 min at a flow rate of 0.2 mL/min with a 2-μL injection volume. The method is validated for linearity, accuracy, repeatability, limits of detection (LOD), and limits of quantification (LOQ). Seven plant samples and 21 dietary supplements claiming to contain Rauwolfia roots were analyzed and content of total alkaloids (1-7) varied, namely, 1.57-12.1 mg/g dry plant material and 0.0-4.5 mg/day, respectively. The results indicated that commercial products are of variable quality. The developed analytical method is simple, economic, fast, and suitable for quality control analysis of Rauwolfia samples and commercial products. The UHPLC-QToF-mass spectrometry with electrospray ionization (ESI) interface method is described for the confirmation and characterization of alkaloids from plant samples. This method involved the detection of M + H or M(+) ions in the positive mode.

摘要

已开发出一种超高效液相色谱-紫外检测法,用于同时分析蛇根木(Rauwolfia serpentina (L.) Benth. ex Kurz.)根样品中的七种生物碱[阿吗灵(1)、育亨宾(2)、柯楠因(3)、阿吗碱(4)、蛇根碱(5)、异蛇根碱(6)和利血平(7)]。采用反相C18色谱柱,以均含有0.05%甲酸的水和乙腈为流动相进行色谱分离。七种化合物在流速为0.2 mL/min、进样量为2 μL的条件下,8分钟内完全分离。该方法在线性、准确度、重复性、检测限(LOD)和定量限(LOQ)方面均经过验证。对七个植物样品和21种声称含有蛇根木根的膳食补充剂进行了分析,总生物碱(1 - 7)的含量各不相同,分别为1.57 - 12.1 mg/g干植物材料和0.0 - 4.5 mg/天。结果表明市售产品质量参差不齐。所开发的分析方法简便、经济、快速,适用于蛇根木样品和市售产品的质量控制分析。描述了采用电喷雾电离(ESI)接口的超高效液相色谱-四极杆飞行时间质谱法对植物样品中的生物碱进行确证和表征。该方法涉及在正模式下检测M + H或M(+)离子。

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