title: One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.
abstract: A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix.
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors.forename: Zheng
authors.initials: Z
authors.lastname: Zhang
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors.forename: Yan-Hong
authors.initials: YH
authors.lastname: Hao
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors.forename: Jun
authors.initials: J
authors.lastname: Ding
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors.forename: Sheng-Nan
authors.initials: SN
authors.lastname: Xu
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
authors.forename: Bi-Feng
authors.initials: BF
authors.lastname: Yuan
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China. Electronic address: yqfeng@whu.edu.cn.
authors.forename: Yu-Qi
authors.initials: YQ
authors.lastname: Feng
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D057930:Click Chemistry / Q000379:methods*; D005875:Gibberellins / Q000032:analysis* / Q000302:isolation & purification; D013058:Mass Spectrometry / Q000379:methods*; D036103:Nanotechnology / Q000379:methods; D012275:Oryza / Q000737:chemistry* / Q000378:metabolism*; D012822:Silicon Dioxide / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods; D013438:Sulfhydryl Compounds / Q000737:chemistry
chemical_list: D005875:Gibberellins; D013438:Sulfhydryl Compounds; D012822:Silicon Dioxide
keywords: Capillary liquid chromatography–mass spectrometry; Derivatization; Gibberellin; Organic-silica hybrid monolithic capillary column; Pipette tip solid phase extraction