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采用蒸发光散射和质谱检测的液相色谱法测定海参中的三萜糖苷。

Determination of the triterpene glycosides in sea cucumbers by liquid chromatography with evaporative light scattering and mass spectrometry detection.

作者信息

Yang Jie, Wang Yuanhong, Zhang Ran, Jiang Tifngfu, Lv Zhihua

机构信息

Key Laboratory of Marine Drugs, School of Medicine and Pharmacy, Ocean University of China, Qingdao, China; Shandong Provincial Key Laboratory of Glycoscience & Glycotechnology, Ocean University of China, Qingdao, China.

出版信息

J Sep Sci. 2015 Apr;38(7):1117-22. doi: 10.1002/jssc.201401253. Epub 2015 Mar 2.

Abstract

Holothurian triterpene glycosides possess various kinds of biological activities, including antifungal, cytotoxic, hemolytic, cytostatic, and immunomodulatory effects. In this study, a rapid extraction method of triterpene glycosides from sea cucumbers using a small column of C18 solid phase was first developed. Furthermore, a novel high-performance liquid chromatography method coupled with evaporative light scattering detection and electrospray ionization mass spectrometry was established for the determination of each triterpene glycosides from different sea cucumbers. Simultaneous separation of all kind of triterpene glycoside were achieved on a C18 column. A gradient of aqueous acetonitrile was applied, and the method was validated. The liquid chromatography method was applied to the online mass detection to identify the triterpene glycosides in the purified extraction of eight kinds of pulverized sea cucumber from the market of Qingdao, China. The negative mode of M-H/M-Na exclusively shown signals corresponding to the triterpene glycosides previously reported and the MS(2) product ions of those ions indicate the specific structure of each triterpene glycoside.

摘要

海参三萜糖苷具有多种生物活性,包括抗真菌、细胞毒性、溶血、细胞抑制和免疫调节作用。在本研究中,首次开发了一种使用C18固相小柱从海参中快速提取三萜糖苷的方法。此外,建立了一种新型的高效液相色谱法,结合蒸发光散射检测和电喷雾电离质谱法,用于测定不同海参中的每种三萜糖苷。在C18柱上实现了所有种类三萜糖苷的同时分离。采用乙腈水溶液梯度洗脱,对该方法进行了验证。将液相色谱法应用于在线质谱检测,以鉴定从中国青岛市场购买的八种粉碎海参的纯化提取物中的三萜糖苷。M-H/M-Na的负离子模式仅显示出与先前报道的三萜糖苷相对应的信号,并且这些离子的MS(2)产物离子表明了每种三萜糖苷的特定结构。

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