Automated and sensitive analysis of 28-epihomobrassinolide in Arabidopsis thaliana by on-line polymer monolith microextraction coupled to liquid chromatography-mass spectrometry. 2013

Xin Wang, and Qiao Ma, and Min Li, and Cuilan Chang, and Yu Bai, and Yuqi Feng, and Huwei Liu
Beijing National Laboratory for Molecular Sciences, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, PR China.

By on-line solid phase microextraction with polymer monolith coupled to liquid chromatography-mass spectrometry (SPME-LC-MS), an automated and sensitive method for analysis of the endogenous 28-epihomobrassinolide (28-epihomoBR) in Arabidopsis thaliana was developed in this work. Firstly, a poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)) monolith was prepared in the capillary and applied in in-tube SPME. Polyethylene glycol (PEG) was used as porogen to adjust the specific surface area and hydrophobicity of the target monolith to get satisfactory permeability, high mechanical strength and good stability. The optimized monolith was then served as extraction medium for analysis of the derivatized 28-epihomoBR in plant samples with the cleanup of matrix and enrichment of desired analyte at the same time. Good linearity was obtained in the linear range of 5-500 ng/L with the coefficient of determination (R(2)) of 0.9996. The limit of detection (S/N=3) of 28-epihomoBR was found to be 2.0 ng/L and the limit of quantification (S/N=10) was 5.0 ng/L. Using this method, the endogenous 0.101 ng/g (FW) 28-epihomoBR was successfully detected from only 400mg A. thaliana samples with satisfactory recovery (80.3-92.1%) and reproducibility (RSD 6.8-9.6%). Comparing with other sample pretreatment methods, this automated on-line SPME-LC-MS method is rapid, sensitive, reproducible and laborsaving.

UI MeSH Term Description Entries
D008689 Methacrylates Acrylic acids or acrylates which are substituted in the C-2 position with a methyl group. Methacrylate
D010936 Plant Extracts Concentrated pharmaceutical preparations of plants obtained by removing active constituents with a suitable solvent, which is evaporated away, and adjusting the residue to a prescribed standard. Herbal Medicines,Plant Extract,Extract, Plant,Extracts, Plant,Medicines, Herbal
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D005026 Ethylene Glycols An ethylene compound with two hydroxy groups (-OH) located on adjacent carbons. They are viscous and colorless liquids. Some are used as anesthetics or hypnotics. However, the class is best known for their use as a coolant or antifreeze. Dihydroxyethanes,Ethanediols,Glycols, Ethylene
D006863 Hydrogen-Ion Concentration The normality of a solution with respect to HYDROGEN ions; H+. It is related to acidity measurements in most cases by pH pH,Concentration, Hydrogen-Ion,Concentrations, Hydrogen-Ion,Hydrogen Ion Concentration,Hydrogen-Ion Concentrations
D013058 Mass Spectrometry An analytical method used in determining the identity of a chemical based on its mass using mass analyzers/mass spectrometers. Mass Spectroscopy,Spectrometry, Mass,Spectroscopy, Mass,Spectrum Analysis, Mass,Analysis, Mass Spectrum,Mass Spectrum Analysis,Analyses, Mass Spectrum,Mass Spectrum Analyses,Spectrum Analyses, Mass
D015203 Reproducibility of Results The statistical reproducibility of measurements (often in a clinical context), including the testing of instrumentation or techniques to obtain reproducible results. The concept includes reproducibility of physiological measurements, which may be used to develop rules to assess probability or prognosis, or response to a stimulus; reproducibility of occurrence of a condition; and reproducibility of experimental results. Reliability and Validity,Reliability of Result,Reproducibility Of Result,Reproducibility of Finding,Validity of Result,Validity of Results,Face Validity,Reliability (Epidemiology),Reliability of Results,Reproducibility of Findings,Test-Retest Reliability,Validity (Epidemiology),Finding Reproducibilities,Finding Reproducibility,Of Result, Reproducibility,Of Results, Reproducibility,Reliabilities, Test-Retest,Reliability, Test-Retest,Result Reliabilities,Result Reliability,Result Validities,Result Validity,Result, Reproducibility Of,Results, Reproducibility Of,Test Retest Reliability,Validity and Reliability,Validity, Face
D017360 Arabidopsis A plant genus of the family BRASSICACEAE that contains ARABIDOPSIS PROTEINS and MADS DOMAIN PROTEINS. The species A. thaliana is used for experiments in classical plant genetics as well as molecular genetic studies in plant physiology, biochemistry, and development. Arabidopsis thaliana,Cress, Mouse-ear,A. thaliana,A. thalianas,Arabidopses,Arabidopsis thalianas,Cress, Mouse ear,Cresses, Mouse-ear,Mouse-ear Cress,Mouse-ear Cresses,thaliana, A.,thaliana, Arabidopsis,thalianas, A.
D052617 Solid Phase Microextraction A solventless sample preparation method, invented in 1989, that uses a fused silica fiber which is coated with a stationary phase. It is used for sample cleanup before using other analytical methods. Microextraction, Solid Phase,Solid Phase Microextractions
D057230 Limit of Detection Concentration or quantity that is derived from the smallest measure that can be detected with reasonable certainty for a given analytical procedure. Limits of Detection,Detection Limit,Detection Limits

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