Rapid screening for bisbibenzyls in bryophyte crude extracts using liquid chromatography/tandem mass spectrometry.
Rapid screening for bisbibenzyls in bryophyte crude extracts using liquid chromatography/tandem mass spectrometry.
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DOI：
10.1002/rcm.3115
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发表时间：
2007-08
期刊：
影响因子：
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通讯作者：
J. Xing;C. Xie;Jian-bo Qu;Huai-fang Guo;Beibei Lv;H. Lou
中科院分区：
文献类型：
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作者：
J. Xing;C. Xie;Jian-bo Qu;Huai-fang Guo;Beibei Lv;H. Lou
建立了一种简单、快速的液相色谱-二极管阵列检测/串联质谱（LC-DAD/MS/MS）定性方法，并验证了该方法的有效性。用乙醇简单提取并用乙醚浓缩分析物后，对提取物进行LC-DAD/MS/MS分析。总仪器周转时间为50分钟，以获得在苯并咪唑中的联苄异构体的基线分离。采用MS全扫描、MS/MS前体离子扫描和MS/MS产物离子扫描模式进行筛选。所研究的联苄标准品的检测限（LOD）等于或低于10 ng/mL。结果还表明，该方法具有可接受的精密度，可用于日常定性鉴别。双联苄基类型，即一个联苯基醚键（A型）、两个联苯基醚键（B型）、一个联苯基醚和一个联苯基键（C型）或其它联苯基类型可以通过它们的ESI-MS/MS产物谱来区分，并且还可以鉴定烷氧基取代基的数目。联苯基和联苯醚键的连接位点不能确定一个未知的bisbibenzyl单独从其质谱。该系统用于支持包括地钱（Marchantia polymorpha L.）中间蕨和狭星壳（Asterella angusta）。其中7/12、8/5和8/9个已确认/未确认的双联苄分别根据其MS/MS数据、UV光谱和保留行为被鉴定。该筛选方法大大减少了定性分析的时间和成本，结构-裂解-UV关系将有助于高通量筛选（HTS）的bisbibenzylcompounds中的briticites。同时也为其它天然产物结构族的测定提供了一种简便的方法。
A simple and rapid qualitative liquid chromatography-diode-array detection/tandem mass spectrometry (LC-DAD/MS/MS) method was developed and validated for screening bisbibenzyl compounds in bryophyte crude extracts at sub-ppm levels. After simple extraction with ethanol and analyte concentration with diethyl ether, the extracts were subjected to LC-DAD/MS/MS analysis. The overall instrument turnaround time was 50 min to obtain baseline separation of bisbibenzyl isomers in bryophytes. MS full scan, MS/MS precursor ion scan and MS/MS product ion scan modes were used for the screening. The bisbibenzyl standards studied gave limits of detection (LODs) at or below 10 ng/mL. The results also indicated that the method had acceptable precision to be used on a day-to-day basis for qualitative identification. The bisbibenzyl types, i.e. one biphenyl ether bond (A-type), two biphenyl ether bonds (B-type), one biphenyl ether and one biphenyl bond (C-type), or other biphenyl types can be differentiated by their ESI-MS/MS product profiles, and the number of alkoxyl substituents can also be identified. The linkage sites of biphenyl and biphenyl ether bonds cannot be identified for an unknown bisbibenzyl solely from its mass spectra. This system was used to support three screening assays of bryophytes including Marchantia polymorpha L., Ptagiochasm intermedium L. and Asterella angusta, which were collected from different places in China. From them, 7/12, 8/5 and 8/9 confirmed/unconfirmed bisbibenzyls were identified, respectively, based on their MS/MS data, UV spectra and the retention behavior. The screening method considerably reduced the time and the cost for the qualitative analyses, and the structure-fragmentation-UV relationships will facilitate the high-throughput screening (HTS) of bisbibenzyl compounds in bryophytes. It is also intended as a simple and convenient way for the determination of other structural families of natural products.