Analysis of primary aromatic amines using precolumn derivatization by HPLC fluorescence detection and online MS identification | |
Zhao, Xianen1,2; Suo, Yourui1 | |
刊名 | journal of separation science |
2008-03-01 | |
卷号 | 31期号:4页码:646-658 |
关键词 | aromatic amines derivatization 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)acetic acid 2-9-acridoneyacetic acid HPLC MS |
合作状况 | 其它 |
中文摘要 | 2-(2-phenyl-1h-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (ppia) and 2-(9-acridone)-acetic acid (aaa), two novel precolumn fluorescent derivatization reagents, have been developed and compared for analysis of primary aromatic amines by high performance liquid chromatographic fluorescence detection coupled with online mass spectrometric identification. ppia and aaa react rapidly and smoothly with the aromatic amines on the basis of a condensation reaction using 1-ethyl-3-(3dimethylaminopropyl)-carbodiimide (edc) as dehydrating catalyst to form stable derivatives with emission wavelengths at 380 and 440 nm, respectively. taking six primary aromatic amines (aniline, 2-methylaniline, 2-methoxyaniline, 4-methylaniline, 4-chloroaniline, and 4-bromoaniline) as testing compounds, derivatization conditions such as coupling reagent, basic catalyst, reaction temperature and time, reaction solvent, and fluorescent labeling reagent concentration have also been investigated. with the better ppia method, chromatographic separation of derivatized aromatic amines exhibited a good baseline resolution on an rp column. at the same time, by online mass spectrometric identification with atmospheric pressure chemical ionization (apci) source in positive ion mode, the ppia-labeled derivatives were characterized by easy-to-interpret mass spectra due to the prominent protonated molecular ion m/z [m + h](+) and specific fragment ions (ms/ms) m/z 335 and 295. the linear range is 24.41 fmol-200.0 pmol with correlation coefficients in the range of 0.9996-0.9999, and detection limits of ppia-labeled aromatic amines are 0.12-0.21 nmol/l (s/n = 3). method repeatability, precision, and recovery were evaluated and the results were excellent for the efficient hplc analysis. the most important argument, however, was the high sensitivity and ease-of-handling of the ppia method. preliminary experiments with wastewater samples collected from the waterspout of a paper mill and its nearby soil where pollution with aromatic amines may be expected show that the method is highly validated with little interference in the chromatogram. |
英文摘要 | 2-(2-phenyl-1h-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (ppia) and 2-(9-acridone)-acetic acid (aaa), two novel precolumn fluorescent derivatization reagents, have been developed and compared for analysis of primary aromatic amines by high performance liquid chromatographic fluorescence detection coupled with online mass spectrometric identification. ppia and aaa react rapidly and smoothly with the aromatic amines on the basis of a condensation reaction using 1-ethyl-3-(3dimethylaminopropyl)-carbodiimide (edc) as dehydrating catalyst to form stable derivatives with emission wavelengths at 380 and 440 nm, respectively. taking six primary aromatic amines (aniline, 2-methylaniline, 2-methoxyaniline, 4-methylaniline, 4-chloroaniline, and 4-bromoaniline) as testing compounds, derivatization conditions such as coupling reagent, basic catalyst, reaction temperature and time, reaction solvent, and fluorescent labeling reagent concentration have also been investigated. with the better ppia method, chromatographic separation of derivatized aromatic amines exhibited a good baseline resolution on an rp column. at the same time, by online mass spectrometric identification with atmospheric pressure chemical ionization (apci) source in positive ion mode, the ppia-labeled derivatives were characterized by easy-to-interpret mass spectra due to the prominent protonated molecular ion m/z [m + h](+) and specific fragment ions (ms/ms) m/z 335 and 295. the linear range is 24.41 fmol-200.0 pmol with correlation coefficients in the range of 0.9996-0.9999, and detection limits of ppia-labeled aromatic amines are 0.12-0.21 nmol/l (s/n = 3). method repeatability, precision, and recovery were evaluated and the results were excellent for the efficient hplc analysis. the most important argument, however, was the high sensitivity and ease-of-handling of the ppia method. preliminary experiments with wastewater samples collected from the waterspout of a paper mill and its nearby soil where pollution with aromatic amines may be expected show that the method is highly validated with little interference in the chromatogram. |
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 ; capillary-zone-electrophoresis ; mass-spectrometry ; 2-(9-anthryl)ethyl chloroformate ; fluorometric detection ; phase microextraction ; environmental waters ; aliphatic-amines ; acids ; derivatives |
收录类别 | SCI |
语种 | 英语 |
WOS记录号 | WOS:000254137900007 |
公开日期 | 2009-12-07 |
内容类型 | 期刊论文 |
源URL | [http://ir.nwipb.ac.cn/handle/363003/1225] |
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 Inst Plateau 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,Suo, Yourui. Analysis of primary aromatic amines using precolumn derivatization by HPLC fluorescence detection and online MS identification[J]. journal of separation science,2008,31(4):646-658. |
APA | Zhao, Xianen,&Suo, Yourui.(2008).Analysis of primary aromatic amines using precolumn derivatization by HPLC fluorescence detection and online MS identification.journal of separation science,31(4),646-658. |
MLA | Zhao, Xianen,et al."Analysis of primary aromatic amines using precolumn derivatization by HPLC fluorescence detection and online MS identification".journal of separation science 31.4(2008):646-658. |
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