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
文献类型：期刊论文
| 作者 | You, Jinmao; Zhao, Wenchen; Liu, Lingjun; Zhao, Xianen; Suo, Yourui; Wang, Honglun; Li, Yulin; Ding, Chenxu |
| 刊名 | talanta
 |
| 出版日期 | 2007-05-15 |
| 卷号 | 72期号:3页码:914-925 |
| 关键词 | derivatization HPLC amines 2-(11H-benzo[a]-carbazol-11-yl) ethyl chloroformate (BCEC-Cl) |
| 合作状况 | 其它 |
| 中文摘要 | 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. |
| 英文摘要 | 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. |
| 学科主题 | 生物科学 |
| WOS标题词 | science & technology ; physical sciences |
| 类目[WOS] | chemistry, analytical |
| 研究领域[WOS] | chemistry |
| 关键词[WOS] | performance liquid-chromatography ; solid-phase microextraction ; secondary aliphatic-amines ; mass-spectrometry ; 9-fluorenylmethyl chloroformate ; precolumn derivatization ; biogenic-amines ; waste-water ; acids ; behavior |
| 收录类别 | SCI |
| 语种 | 英语 |
| WOS记录号 | WOS:000246832000005 |
| 公开日期 | 2009-12-07 |
| 源URL | [http://ir.nwipb.ac.cn/handle/363003/1271]  |
| 专题 | 西北高原生物研究所_中国科学院西北高原生物研究所 |
| 作者单位 | 1.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 |
| 推荐引用方式 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. |
入库方式： OAI收割
来源：西北高原生物研究所
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