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Determination of aliphatic amines from soil and wastewater of a paper mill by pre-column derivatization using HPLC and tandem mass spectrometry (HPLC-MS/MS)
文献类型：期刊论文
| 作者 | Zhao, Xianen; You, Jinmao; Suo, Yourui |
| 刊名 | journal of liquid chromatography & related technologies
 |
| 出版日期 | 2007 |
| 卷号 | 30期号:13-16页码:1963-1979 |
| 关键词 | derivatization aliphatic amines HPLC APCI/MS 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC) fluorescence detection |
| 合作状况 | 其它 |
| 中文摘要 | a pre-column derivatization method for the sensitive determination of aliphatic amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (bceoc) followed by hplc with fluorescence detection and apci/nis identification in positive-ion mode has been developed. the chromophore of 2-(9-carbazole)-ethyl chloroformate (ceoc) reagent was replaced by the 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing reagent, bceoc, that 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](+) with apci/ms in positive-ion mode. the collision induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 264.1, m/z 246.0 and m/z 218.1, corresponding to the cleavages of ch2ch2o-co, ch2ch2-oco, and n-ch2ch2o bonds. studies on derivatization conditions demonstrated that excellent derivatization yields close to 100% were observed with a 3 to 4-fold molar reagent excess in acetonitrile solvent, in the presence of borate buffer (ph 9.0) at 40 degrees c for 10 min. in addition, the detection responses for bceoc derivatives were compared with those obtained with ceoc and fmoc as labeling reagents. the ratios i-bceoc/i-ceoc and i-bceoc/i-fmoc were, respectively, 1.40-2.76 and 1.36-2.92 for fluorescence responses (here, i was the relative fluorescence intensity). separation of the amine derivatives had been optimized on an eclipse xdb-c-8 column. detection limits calculated from an 0.10 pmol injection, at a signal-to-noise ratio of 3, were 18.65-38.82 fmol (injection volume 10 mu l for fluorescence detection. the relative standard deviations for intraday determination (n = 6) of standard amine derivatives (50 pmol) were 0.0063-0.037% for retention times and 3.36-6.93% for peak areas. the mean intra-and inter-assay precision for all amines were <5.4% and 5.8%, respectively. the recoveries of amines ranged from 96 to 113%. excellent linear responses were observed with correlation coefficients of >0.9994. the established method provided a simple and highly sensitive technique for the quantitative analysis of trace amounts of aliphatic amines from biological and natural environmental samples. |
| 英文摘要 | a pre-column derivatization method for the sensitive determination of aliphatic amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (bceoc) followed by hplc with fluorescence detection and apci/nis identification in positive-ion mode has been developed. the chromophore of 2-(9-carbazole)-ethyl chloroformate (ceoc) reagent was replaced by the 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing reagent, bceoc, that 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](+) with apci/ms in positive-ion mode. the collision induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 264.1, m/z 246.0 and m/z 218.1, corresponding to the cleavages of ch2ch2o-co, ch2ch2-oco, and n-ch2ch2o bonds. studies on derivatization conditions demonstrated that excellent derivatization yields close to 100% were observed with a 3 to 4-fold molar reagent excess in acetonitrile solvent, in the presence of borate buffer (ph 9.0) at 40 degrees c for 10 min. in addition, the detection responses for bceoc derivatives were compared with those obtained with ceoc and fmoc as labeling reagents. the ratios i-bceoc/i-ceoc and i-bceoc/i-fmoc were, respectively, 1.40-2.76 and 1.36-2.92 for fluorescence responses (here, i was the relative fluorescence intensity). separation of the amine derivatives had been optimized on an eclipse xdb-c-8 column. detection limits calculated from an 0.10 pmol injection, at a signal-to-noise ratio of 3, were 18.65-38.82 fmol (injection volume 10 mu l for fluorescence detection. the relative standard deviations for intraday determination (n = 6) of standard amine derivatives (50 pmol) were 0.0063-0.037% for retention times and 3.36-6.93% for peak areas. the mean intra-and inter-assay precision for all amines were <5.4% and 5.8%, respectively. the recoveries of amines ranged from 96 to 113%. excellent linear responses were observed with correlation coefficients of >0.9994. the established method provided a simple and highly sensitive technique for the quantitative analysis of trace amounts of aliphatic amines from biological and natural environmental samples. |
| 学科主题 | 生物化学 |
| WOS标题词 | science & technology ; life sciences & biomedicine ; physical sciences |
| 类目[WOS] | biochemical research methods ; chemistry, analytical |
| 研究领域[WOS] | biochemistry & molecular biology ; chemistry |
| 关键词[WOS] | performance liquid-chromatography ; solid-phase microextraction ; 9-fluorenylmethyl chloroformate ; fluorescence detection ; reagent ; acids ; methanol ; chloride |
| 收录类别 | SCI |
| 语种 | 英语 |
| WOS记录号 | WOS:000248539300009 |
| 公开日期 | 2009-12-07 |
| 源URL | [http://ir.nwipb.ac.cn/handle/363003/1263]  |
| 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.Chinese Acad Sci, NW Plateau Inst Biol, Xining 810001, Peoples R China 2.Chinese Acad Sci, Grad Sch, Beijing, Peoples R China |
| 推荐引用方式 GB/T 7714 | Zhao, Xianen,You, Jinmao,Suo, Yourui. Determination of aliphatic amines from soil and wastewater of a paper mill by pre-column derivatization using HPLC and tandem mass spectrometry (HPLC-MS/MS)[J]. journal of liquid chromatography & related technologies,2007,30(13-16):1963-1979. |
| APA | Zhao, Xianen,You, Jinmao,&Suo, Yourui.(2007).Determination of aliphatic amines from soil and wastewater of a paper mill by pre-column derivatization using HPLC and tandem mass spectrometry (HPLC-MS/MS).journal of liquid chromatography & related technologies,30(13-16),1963-1979. |
| MLA | Zhao, Xianen,et al."Determination of aliphatic amines from soil and wastewater of a paper mill by pre-column derivatization using HPLC and tandem mass spectrometry (HPLC-MS/MS)".journal of liquid chromatography & related technologies 30.13-16(2007):1963-1979. |
入库方式： OAI收割
来源：西北高原生物研究所
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