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采用液相色谱 - 质谱联用和自由基清除法对五味子经改良超声和超临界流体提取物中苯并[a,c]环辛二烯木脂素进行高通量筛选及抗氧化测定

High throughput screening and antioxidant assay of dibenzo[a,c]cyclooctadiene lignans in modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill by liquid chromatography--mass spectrometry and a free radical-scavenging method.

作者信息

Wang Ming-Chih, Lai Yih-Cherng, Chang Chia-Lin

机构信息

Graduate School of Biotechnology, HungKuang University, Taichung, Taiwan, ROC.

出版信息

J Sep Sci. 2008 May;31(8):1322-32. doi: 10.1002/jssc.200700443.

DOI:10.1002/jssc.200700443
PMID:18446887
Abstract

Dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill are well known because of their hepatoprotective activity, antioxidant activity, and anticancer effect. For the isolation of the dibenzo[a,c]cyclooctadiene lignans of Schisandra chinensis Baill two extraction methods were used: modified-ultrasonic extraction and supercritical fluid extraction. A specific and fast analytical method for structure identification is established for quality control because structure elucidation could be accomplished by means of liquid chromatography-mass spectrometry (LC-MS) technologies. The separation and identification of the compounds were completed by: (i) a water-acetonitrile gradient system using a C18 reversed-phase column; (ii) UV detection at 225 nm; (iii) MS/MS experiments with electrospray ionization interface (ESI) ion trap mass spectrometry in the positive mode. Normalized collision energy was used to obtain fragment ions of structural relevance in the LC-MS/MS. These results provided a reliable LC-MS/MS method for the determination of the dibenzo[a,c]cyclooctadiene lignans from Schisandra chinensis Baill. Finally, we also detected 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging effects (%) of the modified-ultrasonic and supercritical fluid extracts of Schisandra chinensis Baill compared with 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox). The antioxidant activities of the modified-ultrasonic and supercritical fluid extracts were lower than that of trolox.

摘要

五味子中的二苯并[a,c]环辛二烯木脂素因其保肝活性、抗氧化活性和抗癌作用而闻名。为了分离五味子中的二苯并[a,c]环辛二烯木脂素,采用了两种提取方法:改良超声提取法和超临界流体萃取法。由于可以通过液相色谱-质谱(LC-MS)技术完成结构解析,因此建立了一种用于质量控制的特定且快速的结构鉴定分析方法。化合物的分离和鉴定通过以下方式完成:(i)使用C18反相柱的水-乙腈梯度系统;(ii)在225nm处进行紫外检测;(iii)采用电喷雾电离接口(ESI)离子阱质谱在正模式下进行MS/MS实验。在LC-MS/MS中使用归一化碰撞能量来获得具有结构相关性的碎片离子。这些结果为测定五味子中的二苯并[a,c]环辛二烯木脂素提供了一种可靠的LC-MS/MS方法。最后,我们还检测了五味子改良超声提取物和超临界流体提取物对1,1-二苯基-2-苦基肼(DPPH)的清除率(%),并与6-羟基-2,5,7,8-四甲基色满-2-羧酸(Trolox)进行了比较。改良超声提取物和超临界流体提取物的抗氧化活性均低于Trolox。

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