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4-(1-METHYL-1H-PHENANTHRO[9,10-d]IMIDAZOLE-2-) BENZOIC ACID (MPIBA) AND ITS APPLICATION FOR DETERMINATION OF AMINES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH FLUORESCENCE DETECTION AND IDENTIFICATION WITH MASS SPECTROSCOPY/ATMOSPHERIC PRESSURE CHEMICAL IONIZATION
Xia Lian1,2,3; Sun Zhiwei2,3; Suo Yourui2; You Jinmao1,2
2010
发表期刊JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
ISSN1082-6076
卷号33期号:1页码:72-88
文章类型Article
摘要A simple, sensitive, and mild method for the determination of amines based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC center dot HCl) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acid amides with labeling reagent 4-s(1-methyl-1H-phenanthro[9,10-d]imidazole-2-) benzoic acid (MPIBA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in acetonitrile to give the corresponding sensitively fluorescent derivatives with a maximum excitation at ex 260nm and a maximum emission at em 446nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH]+ under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C8 column. Liquid chromatography separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 90.00pmol to 88fmol injection, at a signal-to-noise ratio of 3, were 10.5-53.4fmol. Excellent linear responses were observed with coefficients of 0.9996. The established method for the determination of aliphatic amines from real wastewater was satisfactory.; A simple, sensitive, and mild method for the determination of amines based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC center dot HCl) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acid amides with labeling reagent 4-s(1-methyl-1H-phenanthro[9,10-d]imidazole-2-) benzoic acid (MPIBA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in acetonitrile to give the corresponding sensitively fluorescent derivatives with a maximum excitation at ex 260nm and a maximum emission at em 446nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH]+ under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C8 column. Liquid chromatography separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 90.00pmol to 88fmol injection, at a signal-to-noise ratio of 3, were 10.5-53.4fmol. Excellent linear responses were observed with coefficients of 0.9996. The established method for the determination of aliphatic amines from real wastewater was satisfactory.
关键词4-(1-methyl-1h-phenanthro[9 10-d]Imidazole-2-) Benzoic Acid (Mpiba) Amines Determination Fluorescence Detection Hplc Mass Spectrometry
WOS标题词Science & Technology ; Life Sciences & Biomedicine ; Physical Sciences
关键词[WOS]ALIPHATIC-AMINES ; BIOGENIC-AMINES ; DERIVATIZATION ; SPECTROMETRY ; METHANOL ; SERUM
收录类别SCI
语种英语
WOS研究方向Biochemistry & Molecular Biology ; Chemistry
WOS类目Biochemical Research Methods ; Chemistry, Analytical
WOS记录号WOS:000272680200006
引用统计
被引频次:1[WOS]   [WOS记录]     [WOS相关记录]
文献类型期刊论文
条目标识符http://210.75.249.4/handle/363003/1780
专题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, Key Lab Life Organ Anal Shan Dong Prov, Qufu 273165, Shandong, Peoples R China
2.Chinese Acad Sci, NW Plateau Inst Biol, Xining, Peoples R China
3.Chinese Acad Sci, Grad Univ, Beijing, Peoples R China
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GB/T 7714
Xia Lian,Sun Zhiwei,Suo Yourui,et al. 4-(1-METHYL-1H-PHENANTHRO[9,10-d]IMIDAZOLE-2-) BENZOIC ACID (MPIBA) AND ITS APPLICATION FOR DETERMINATION OF AMINES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH FLUORESCENCE DETECTION AND IDENTIFICATION WITH MASS SPECTROSCOPY/ATMOSPHERIC PRESSURE CHEMICAL IONIZATION[J]. JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,2010,33(1):72-88.
APA Xia Lian,Sun Zhiwei,Suo Yourui,&You Jinmao.(2010).4-(1-METHYL-1H-PHENANTHRO[9,10-d]IMIDAZOLE-2-) BENZOIC ACID (MPIBA) AND ITS APPLICATION FOR DETERMINATION OF AMINES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH FLUORESCENCE DETECTION AND IDENTIFICATION WITH MASS SPECTROSCOPY/ATMOSPHERIC PRESSURE CHEMICAL IONIZATION.JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,33(1),72-88.
MLA Xia Lian,et al."4-(1-METHYL-1H-PHENANTHRO[9,10-d]IMIDAZOLE-2-) BENZOIC ACID (MPIBA) AND ITS APPLICATION FOR DETERMINATION OF AMINES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH FLUORESCENCE DETECTION AND IDENTIFICATION WITH MASS SPECTROSCOPY/ATMOSPHERIC PRESSURE CHEMICAL IONIZATION".JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES 33.1(2010):72-88.
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