Identification and determination of the major constituents in Traditional Chinese Medicinal formula Danggui-Shaoyao-San by HPLC-DAD-ESI-MS/MS
Identification and determination of the major constituents in Traditional Chinese Medicinal formula Danggui-Shaoyao-San by HPLC-DAD-ESI-MS/MS
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DOI：
10.1016/j.jpba.2009.03.039
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发表时间：
2009-09-08
影响因子：
3.4
通讯作者：
Yu, Boyang
中科院分区：
文献类型：
--
作者：
Chen, Linlin;Qi, Jin;Yu, Boyang
当归芍药散是由当归、川芎、当归、白术、泽泻等六味药组成的传统中药方剂，是我国传统的妇科经典方剂。然而，其活性物质仍然未知。本文建立了HPLC/DAD/ESI-MS/MS法对DSS中的主要成分进行定性和定量分析。提出了参比化合物的ESI-MS/MS裂解行为，用于辅助DSS提取物中组分的结构鉴定。通过对41个化合物的保留时间、紫外光谱和质谱与文献数据的比较，鉴定或初步鉴定了单萜苷类、酚酸类、酞内酯类、倍半萜类和三萜类等化合物，其中14个化合物的结构与文献数据一致（没食子酸、芍药苷、芍药苷、阿魏酸、苯甲酸、川芎素1、阿魏酸松柏酯、川芎素A、3-丁基苯酞、Z-藁本内酯、采用高效液相色谱-二极管阵列检测器（HPLC-DAD），以乙腈/水-甲酸（100：0.1，v/v）为流动相，采用C-18色谱柱，流动相为乙腈/水-甲酸（100：0.1，v/v）进行梯度洗脱。对定量方法的线性、精密度、准确度、检测限和定量限进行了验证，证明该方法灵敏、准确、重现性好。本研究为DSS提取物及制剂的质量控制提供了依据。(C)2009爱思唯尔有限公司版权所有。
Danggui-Shaoyao-San (DSS), a famous traditional Chinese medicine formula consisting of six herbal medicines (Paeonia lactiflora, Angelica sinensis, Ligusticum chuanxiong, Poria cocos, Atractylodis macro-cephalae and Rhizoma Alismatis), has been used as a classical gynecological remedy in China for centuries. However, its active substances have remained unknown. In this paper, an HPLC/DAD/ESI-MS/MS method was developed for the qualitative and quantitative analysis of the major constituents in DSS. The ESI-MS/MS fragmentation behavior of the reference compounds was proposed for aiding the structural identification of components in DSS extract. Forty-one compounds including monoterpene glycosides, phenolic acids, phathalides, sesquiterpenoids and triterpenes were identified or tentatively characterized by comparing their retention times, UV and MS spectra with those of authentic compounds or literature data, and 14 of them (gallic acid, albiflorin, paeoniflorin, ferulic acid, benzoic acid, senkyunolide 1, coniferyl ferulate, senkyunolide A, 3-butylphthalide, Z-ligustilide, Z-butylidenephthalide, atractylcnolide II, atractylcnolide I and levistolide A) were determined by HPLC-DAD using a C-18 column and gradient elution of acetonitrile/water-formic acid (100:0.1, v/v). The linearity, precision, accuracy, LOD and LOQ were validated for the quantification method, which proved sensitive, accurate and reproducible. The study might provide a basis for the quality control of DSS extracts and preparations. (C) 2009 Elsevier B.V. All rights reserved.