NWIPB OpenIR
Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS
You, Jinmao; Zhao, Wenchen; Liu, Lingjun; Zhao, Xianen; Suo, Yourui; Wang, Honglun; Li, Yulin; Ding, Chenxu
2007-05-15
Source PublicationTALANTA
Volume72Issue:3Pages:914-925
SubtypeArticle
AbstractA pre-column derivatization method for the sensitive determination of amines using a labeling reagent 2-(11H-benzo[a]-carbazol-11-yl) ethyl chloroformate (BCEC-Cl) followed by high-performance, liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by LC/APCI/MS in positive-ion mode. The chromophore of 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) reagent was replaced by 2-(11H-benzo[a]-carbazol-11-yl) ethyl functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEC-Cl. BCEC-Cl could easily and quickly label amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+ H](+) under APCI/MS in positive-ion mode. The collision-induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 261.8 and m/z 243.8 corresponding to the cleavages of CH2O-CO and CH2-OCO bonds. Studies on derivatization demonstrated excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% were observed with three- to four-fold molar reagent excess. In addition, the detection responses for BCEC-derivatives were compared to those obtained using 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) and 9-fluorenyl methylchloroformate, (FMOC-Cl) as labeling reagents. The ratios I-BCEC/I-BCEOC = 1.94-2.17 and I-BCEC/I-FMOC = 1.04-2.19 for fluorescent (FL) responses (here, I was relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits calculated from 0.50 pmol injection, at a signal-to-noise ratio of 3, were 1.77-14.4 fmol. The relative standard deviations for within-day determination (n = 11) were 1.84-2.89% for the tested amines. The mean intra- and inter-assay precision for all amines levels were < 3.64% and 2.52%, respectively. The mean recoveries ranged from 96.6% to 107.1% with their standard deviations in the range of 0.8-2.7. Excellent linear responses were observed with coefficients of > 0.9996. (C) 2006 Elsevier B.V. All rights reserved.; A pre-column derivatization method for the sensitive determination of amines using a labeling reagent 2-(11H-benzo[a]-carbazol-11-yl) ethyl chloroformate (BCEC-Cl) followed by high-performance, liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by LC/APCI/MS in positive-ion mode. The chromophore of 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) reagent was replaced by 2-(11H-benzo[a]-carbazol-11-yl) ethyl functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEC-Cl. BCEC-Cl could easily and quickly label amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+ H](+) under APCI/MS in positive-ion mode. The collision-induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 261.8 and m/z 243.8 corresponding to the cleavages of CH2O-CO and CH2-OCO bonds. Studies on derivatization demonstrated excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% were observed with three- to four-fold molar reagent excess. In addition, the detection responses for BCEC-derivatives were compared to those obtained using 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) and 9-fluorenyl methylchloroformate, (FMOC-Cl) as labeling reagents. The ratios I-BCEC/I-BCEOC = 1.94-2.17 and I-BCEC/I-FMOC = 1.04-2.19 for fluorescent (FL) responses (here, I was relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits calculated from 0.50 pmol injection, at a signal-to-noise ratio of 3, were 1.77-14.4 fmol. The relative standard deviations for within-day determination (n = 11) were 1.84-2.89% for the tested amines. The mean intra- and inter-assay precision for all amines levels were < 3.64% and 2.52%, respectively. The mean recoveries ranged from 96.6% to 107.1% with their standard deviations in the range of 0.8-2.7. Excellent linear responses were observed with coefficients of > 0.9996. (C) 2006 Elsevier B.V. All rights reserved.
KeywordDerivatization Hplc Amines 2-(11h-benzo[a]-carbazol-11-yl) Ethyl Chloroformate (Bcec-cl)
WOS HeadingsScience & Technology ; Physical Sciences
Subject Area生物科学
WOS KeywordPERFORMANCE LIQUID-CHROMATOGRAPHY ; SOLID-PHASE MICROEXTRACTION ; SECONDARY ALIPHATIC-AMINES ; MASS-SPECTROMETRY ; 9-FLUORENYLMETHYL CHLOROFORMATE ; PRECOLUMN DERIVATIZATION ; BIOGENIC-AMINES ; WASTE-WATER ; ACIDS ; BEHAVIOR
Indexed BySCI
Language英语
WOS Research AreaChemistry
WOS SubjectChemistry, Analytical
WOS IDWOS:000246832000005
Citation statistics
Cited Times:20[WOS]   [WOS Record]     [Related Records in WOS]
Document Type期刊论文
Identifierhttp://210.75.249.4/handle/363003/1271
Collection中国科学院西北高原生物研究所
Affiliation1.Qufu Normal Univ, Coll Chem Sci, Qufu 273165, Shandong, Peoples R China
2.Chinese Acad Sci, NW Plateau Inst Biol, Xining 810001, Peoples R China
Recommended Citation
GB/T 7714
You, Jinmao,Zhao, Wenchen,Liu, Lingjun,et al. Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS[J]. TALANTA,2007,72(3):914-925.
APA You, Jinmao.,Zhao, Wenchen.,Liu, Lingjun.,Zhao, Xianen.,Suo, Yourui.,...&Ding, Chenxu.(2007).Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS.TALANTA,72(3),914-925.
MLA You, Jinmao,et al."Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS".TALANTA 72.3(2007):914-925.
Files in This Item: Download All
File Name/Size DocType Version Access License
Determination of ami(625KB) 开放获取LicenseView Download
Related Services
Recommend this item
Bookmark
Usage statistics
Export to Endnote
Google Scholar
Similar articles in Google Scholar
[You, Jinmao]'s Articles
[Zhao, Wenchen]'s Articles
[Liu, Lingjun]'s Articles
Baidu academic
Similar articles in Baidu academic
[You, Jinmao]'s Articles
[Zhao, Wenchen]'s Articles
[Liu, Lingjun]'s Articles
Bing Scholar
Similar articles in Bing Scholar
[You, Jinmao]'s Articles
[Zhao, Wenchen]'s Articles
[Liu, Lingjun]'s Articles
Terms of Use
No data!
Social Bookmark/Share
File name: Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI MS.pdf
Format: Adobe PDF
All comments (0)
No comment.
 

Items in the repository are protected by copyright, with all rights reserved, unless otherwise indicated.