PMID- 27072523
OWN - NLM
STAT- MEDLINE
DCOM- 20170421
LR  - 20181202
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1446
DP  - 2016 May 13
TI  - Determination of endogenous brassinosteroids using sequential magnetic solid 
      phase extraction followed by in situ derivatization/desorption method coupled 
      with liquid chromatography-tandem mass spectrometry.
PG  - 103-13
LID - S0021-9673(16)30415-0 [pii]
LID - 10.1016/j.chroma.2016.04.012 [doi]
AB  - In this study, a sequential magnetic solid phase extraction followed by in situ 
      derivatization/desorption method was proposed for the fast, selective and 
      sensitive determination of brassinosteroids (BRs) in plant tissues. Magnetic 
      sorbent for quick, easy, cheap, effective, rugged and safe method (mQuEChERS) and 
      polymer(4-vinylphenylboronic acid-co-ethylene glycol dimethacrylate) coated 
      Fe3O4@SiO2 (p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2) were prepared and 
      characterized. Using them as sorbents, pigments and hydrophilic interferents were 
      firstly removed from plant extract by mQuEChERS, and then endogenous BRs were 
      selectively enriched by p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2 through boronate 
      affinity interaction. After loading BRs on p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2, 
      instead of directly eluting free BRs, the adsorbed BRs were released by adding 
      4-(N,N-dimethyamino)phenylboronic acid (4-DMAPBA) solution for in situ 
      derivatizaiton/desorption of BRs based on a transesterification reaction between 
      the boronate moieties of p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2 and 4-DMAPBA, 
      finally the resultant solution was submitted to LC-MS/MS for quantification. The 
      whole procedure of the sequential MSPE could be accomplished within 1h, and the 
      matrix effect to MS signal after the sample pretreatment was estimated to be in 
      the range of 93.0-97.4%. The established method provided broad linear dynamics 
      ranges (1.0-100.0pg/mL) with correlation coefficients (R) >0.9978, substantial 
      sensitivity (limits of detection ranged from 0.27 to 1.29pg/mL), high 
      reproducibility (intra-day and inter-day relative standard deviations (RSDs) less 
      than 14.8%) and satisfactory accuracy (recoveries ranged from 74.0%-116.6%). 
      Furthermore, endogenous BRs were successfully detected in one flower of Brassica 
      napus L. (22.5-542.7pg/g fresh weight) and other plant tissues (13.7-289.8pg/g 
      fresh weight).
CI  - Copyright (c) 2016 Elsevier B.V. All rights reserved.
FAU - Ding, Jun
AU  - Ding J
AD  - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of 
      Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
FAU - Mao, Li-Jing
AU  - Mao LJ
AD  - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of 
      Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
FAU - Guo, Ning
AU  - Guo N
AD  - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of 
      Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
FAU - Yu, Lei
AU  - Yu L
AD  - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of 
      Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
FAU - Feng, Yu-Qi
AU  - Feng YQ
AD  - Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of 
      Education), Department of Chemistry, Wuhan University, Wuhan 430072, China. 
      Electronic address: yqfeng@whu.edu.cn.
LA  - eng
PT  - Journal Article
DEP - 20160404
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Acrylic Resins)
RN  - 0 (Brassinosteroids)
RN  - 0 (Magnetite Nanoparticles)
RN  - 0 (Plant Extracts)
RN  - 0 (Polyvinyls)
RN  - 7631-86-9 (Silicon Dioxide)
SB  - IM
MH  - Acrylic Resins/*chemistry
MH  - Arabidopsis/*chemistry
MH  - Brassica napus/*chemistry
MH  - Brassinosteroids/*analysis
MH  - Chromatography, High Pressure Liquid/methods
MH  - *Magnetite Nanoparticles
MH  - Oryza/*chemistry
MH  - Plant Extracts/chemistry
MH  - Polyvinyls/*chemistry
MH  - Reproducibility of Results
MH  - *Silicon Dioxide
MH  - Solid Phase Extraction
MH  - Tandem Mass Spectrometry/methods
OTO - NOTNLM
OT  - Brassinosteriod
OT  - In situ derivatization/desorption
OT  - LC-MS/MS
OT  - Sequential MSPE
EDAT- 2016/04/14 06:00
MHDA- 2017/04/22 06:00
CRDT- 2016/04/14 06:00
PHST- 2016/02/02 00:00 [received]
PHST- 2016/03/31 00:00 [revised]
PHST- 2016/04/04 00:00 [accepted]
PHST- 2016/04/14 06:00 [entrez]
PHST- 2016/04/14 06:00 [pubmed]
PHST- 2017/04/22 06:00 [medline]
AID - S0021-9673(16)30415-0 [pii]
AID - 10.1016/j.chroma.2016.04.012 [doi]
PST - ppublish
SO  - J Chromatogr A. 2016 May 13;1446:103-13. doi: 10.1016/j.chroma.2016.04.012. Epub 
      2016 Apr 4.