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题名: Quantification of endogenous brassinosteroids in plant by on-line two-dimensional microscale solid phase extraction-on column derivatization coupled with high performance liquid chromatography-tandem mass spectrometry
作者: Wu, Qian1, 2;  Wu, Dapeng1;  Shen, Zheng1;  Duan, Chunfeng1;  Guan, Yafeng1
关键词: On-line two-dimensional microscale solid phase extraction (2D mu SPE) ;  On-column derivatization (OCD) ;  Endogenous brassinosteroids (BRs) ;  Tomato leaf sample
刊名: JOURNAL OF CHROMATOGRAPHY A
发表日期: 2013-07-05
DOI: 10.1016/j.chroma.2013.04.043
卷: 1297, 页:56-63
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology ;  Life Sciences & Biomedicine ;  Physical Sciences
类目[WOS]: Biochemical Research Methods ;  Chemistry, Analytical
研究领域[WOS]: Biochemistry & Molecular Biology ;  Chemistry
英文摘要: An on-line two-dimensional microscale solid phase extraction (2D mu SPE)-on column derivatization (OCD)-high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) method was developed for quantification of brassinosteroids (BRs) in plant tissues. Five BRs with widest distribution in plant species and high bioactivity (24-epibrassinolide,24-epicastasterone, 6-deoxo-24-epicastasterone, teasterone and typhastero) were selected as target analytes. 2D mu SPE column packed sequentially with phenyl boronic acid silica sorbent (the first dimension) and C18 silica sorbent (the second dimension) was used to selectively extract and enrich BRs by 110-146 times. OCD was carried out on the second dimension of 2D mu SPE column with m-aminophenylboronic acid (m-APBA) as a derivatization reagent, enhancing the sensitivity of MS/MS to BRs by 13-8437 times. It was also found that pre-trap of derivatization reagent on the C18 section of 2D mu SPE column could increase reaction efficiency by 3-10 times. The whole process time of the on-line system was less than 30 min. The detection limits of the method for five BRs were between 1.4 and 6.6 pg with RSDs less than 10%. Endogeneous BRs in tomato leaves were analyzed by using this method. Owing to the high selectivity of this on-line 2D mu SPE system, BRs in plant extracts could be quantified using matrix-free standard calibration method with relative recoveries in the range of 80-124%. (C) 2013 Elsevier B.V. All rights reserved.
关键词[WOS]: GAS-CHROMATOGRAPHY ;  ACID
语种: 英语
WOS记录号: WOS:000320821900007
Citation statistics: 
内容类型: 期刊论文
URI标识: http://cas-ir.dicp.ac.cn/handle/321008/137747
Appears in Collections:中国科学院大连化学物理研究所_期刊论文

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作者单位: 1.Chinese Acad Sci, Dalian Inst Chem Phys, Dept Instrumentat & Analyt Chem, Key Lab Separat Sci Analyt Chem CAS, Dalian 116023, Peoples R China
2.Chinese Acad Sci, Dalian Inst Chem Phys, Grad Sch, Beijing 100039, Peoples R China

Recommended Citation:
Wu, Qian,Wu, Dapeng,Shen, Zheng,et al. Quantification of endogenous brassinosteroids in plant by on-line two-dimensional microscale solid phase extraction-on column derivatization coupled with high performance liquid chromatography-tandem mass spectrometry[J]. JOURNAL OF CHROMATOGRAPHY A,2013,1297:56-63.
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