Analysis of mexicanolide- and phragmalin-type limonoids from Heynea trijuga using high-performance liquid chromatography/electrospray tandem mass spectrometry.
Analysis of mexicanolide- and phragmalin-type limonoids from Heynea trijuga using high-performance liquid chromatography/electrospray tandem mass spectrometry.
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DOI：
10.1002/rcm.6563
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发表时间：
2013-06
期刊：
影响因子：
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通讯作者：
Wei Yang;Dong-mei Fang;Hong-ping He;X. Hao;Zhijun Wu;Guo-lin Zhang
中科院分区：
文献类型：
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作者：
Wei Yang;Dong-mei Fang;Hong-ping He;X. Hao;Zhijun Wu;Guo-lin Zhang
柠檬苦素类化合物是一类四氢三萜类化合物，具有多种生物学效应，包括作为有效的拒食剂和昆虫生长调节剂来防治各种害虫。用碰撞诱导解离串联质谱仪(CID-MS/MS)分析佛手莲类和墨西哥内酯类柠檬苦素尚未见报道。方法建立了高效液相色谱/电喷雾电离(HPLC/ESI)-MS/MS联用方法，研究了9种参比芦荟内酯类柠檬苦素的[M+NH4](+)离子的裂解规律。该方法还可用于海棠植物提取物中柠檬苦素类化合物的鉴定。结果侧链丢失和呋喃部分是主要的碎裂形式。然而，由于相同的碎裂途径，产物离子的相对丰度存在差异。在海棠植物提取物中共检测到89个芦荟素和墨西哥内酯类柠檬苦素类化合物，其中50个化合物根据元素组成、裂解途径和参比化合物的主要产物离子谱进行了鉴定或初步表征。此外，还可以初步区分异构体。结论建立了HPLC/ESI-MS/MS方法，可同时鉴定和筛选海棠植物提取物中的芦荟素类和墨西哥内酯类柠檬苦素类化合物。
RATIONALE Limonoids, a class of tetranortriterpenoids, exhibit various biological effects, including acting as potent antifeedants and insect growth-regulators against various pests. The analysis of phragmalin- and mexicanolide-type limonoids by collision-induced dissociation tandem mass spectrometry (CID-MS/MS) has not been reported. METHODS A high-performance liquid chromatography/electrospray ionization (HPLC/ESI)-MS/MS method was developed to investigate the fragmentation patterns of [M+NH4 ](+) ions for nine reference phragmalin- and mexicanolide-type limonoids. The method was also used in the identification of limonoid compounds in botanic extracts of Heynea trijuga. RESULTS The losses of side chains and the furan part were the major fragmentation patterns. However, there was variation in the relative abundances of product ions resulting from the same fragmentation pathways. A total of 89 phragmalin- and mexicanolide-type limonoids in botanic extracts of Heynea trijuga were detected and 50 of these compounds were identified or tentatively characterized based on elemental constituents, fragmentation pathways, and the profile of the major product ions of reference compounds. In addition, the isomers could be tentatively distinguished. CONCLUSIONS An HPLC/ESI-MS/MS method was developed and could be used to simultaneously identify and screen phragmalin- and mexicanolide-type limonoids in botanic extracts of Heynea trijuga.