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采用在线 TLC-DART-MS 对五味子果实中的主要二苯并环辛烷木脂素进行定量分析。

Quantitative analysis of major dibenzocyclooctane lignans in Schisandrae fructus by online TLC-DART-MS.

机构信息

Kyung Hee East-West Pharmaceutical Research Institute, College of Pharmacy, Kyung Hee University, Seoul 130-701, Korea.

出版信息

Phytochem Anal. 2011 May-Jun;22(3):258-62. doi: 10.1002/pca.1273. Epub 2010 Oct 26.

Abstract

INTRODUCTION

Direct analysis in real time (DART) ion source is a powerful ionising technique for the quick and easy detection of various organic molecules without any sample preparation steps, but the lack of quantitation capacity limits its extensive use in the field of phytochemical analysis.

OBJECTIVE

To improvise a new system which utilize DART-MS as a hyphenated detector for quantitation.

METHODOLOGY

A total extract of Schisandra chinensis fruit was analyzed on a TLC plate and three major lignan compounds were quantitated by three different methods of UV densitometry, TLC-DART-MS and HPLC-UV to compare the efficiency of each method. To introduce the TLC plate into the DART ion source at a constant velocity, a syringe pump was employed. The DART-MS total ion current chromatogram was recorded for the entire TLC plate. The concentration of each lignan compound was calculated from the calibration curve established with standard compound.

RESULTS

Gomisin A, gomisin N and schisandrin were well separated on a silica-coated TLC plate and the specific ion current chromatograms were successfully acquired from the TLC-DART-MS system. The TLC-DART-MS system for the quantitation of natural products showed better linearity and specificity than TLC densitometry, and consumed less time and solvent than conventional HPLC method.

CONCLUSION

A hyphenated system for the quantitation of phytochemicals from crude herbal drugs was successfully established. This system was shown to have a powerful analytical capacity for the prompt and efficient quantitation of natural products from crude drugs.

摘要

简介

实时直接分析(DART)离子源是一种强大的电离技术,可快速、轻松地检测各种有机分子,无需任何样品制备步骤,但缺乏定量能力限制了其在植物化学分析领域的广泛应用。

目的

即兴创作一个新系统,利用 DART-MS 作为联检定量检测器。

方法

对五味子果实的总提取物进行 TLC 板分析,并通过三种不同的方法(UV 分光光度法、TLC-DART-MS 和 HPLC-UV)对三种主要木脂素化合物进行定量,以比较每种方法的效率。为了以恒定速度将 TLC 板引入 DART 离子源,使用了注射器泵。记录整个 TLC 板的 DART-MS 总离子电流色谱图。从用标准化合物建立的校准曲线计算每个木脂素化合物的浓度。

结果

五味子甲素、五味子乙素和五味子素在涂覆硅胶的 TLC 板上得到很好的分离,并且成功地从 TLC-DART-MS 系统中获得了特定的离子电流色谱图。TLC-DART-MS 系统用于天然产物的定量显示出比 TLC 密度法更好的线性和特异性,并且比传统的 HPLC 方法消耗更少的时间和溶剂。

结论

成功建立了用于粗草药中植物化学物质定量的联检系统。该系统具有强大的分析能力,可快速、高效地定量粗药中的天然产物。

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