Knowledge Management System of Northwest Institute of Plateau Biology, CAS
Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS | |
You, JM; Chen, XM; Zhao, XN; Su, YR; Wang, HL; Li, YL; Sun, J | |
2006-04-01 | |
发表期刊 | CHROMATOGRAPHIA |
卷号 | 63期号:7-8页码:337-343 |
文章类型 | Article |
摘要 | A pre-column derivatization method for the sensitive determination of amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate (BCIC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives is carried out by high performance liquid chromatography/atmospheric pressure chemical ionization (LC-APCl-MS-MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent is replaced by 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl functional group, which results in a sensitive fluorescence derivatizing reagent BCIC-Cl. BCIC-Cl can easily and quickly label amines. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography and show an intense protonated molecular ion corresponding m/z [MH](+) under APCl in positive-ion mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 260 corresponding to the cleavage of CH2-OCO bond. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% are observed with a 3 to 4-fold molar reagent excess. In addition, the detection responses for BCIC derivatives are compared with those obtained using CEOC and FMOC as derivatization reagents. The ratios of l(BCIC)/l(CEOC) and l(BCIC)/l(FMOC) are, respectively, 1.23-3.14 and 1.25-3.08 for fluorescent (FL) responses (here, l is relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits are calculated from 1.0 pmol injection, at a signal-to-noise ratio of 3, are 10.6-37.8 fmol. The mean interday accuracy ranges from 94 to 105% for fluorescence detection with the largest mean %CV < 7.5. The mean interday precision for all standards is < 6.0% of the expected concentration. Excellent linear responses are observed with coefficients of > 0.9997.; A pre-column derivatization method for the sensitive determination of amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate (BCIC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives is carried out by high performance liquid chromatography/atmospheric pressure chemical ionization (LC-APCl-MS-MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent is replaced by 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl functional group, which results in a sensitive fluorescence derivatizing reagent BCIC-Cl. BCIC-Cl can easily and quickly label amines. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography and show an intense protonated molecular ion corresponding m/z [MH](+) under APCl in positive-ion mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 260 corresponding to the cleavage of CH2-OCO bond. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% are observed with a 3 to 4-fold molar reagent excess. In addition, the detection responses for BCIC derivatives are compared with those obtained using CEOC and FMOC as derivatization reagents. The ratios of l(BCIC)/l(CEOC) and l(BCIC)/l(FMOC) are, respectively, 1.23-3.14 and 1.25-3.08 for fluorescent (FL) responses (here, l is relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits are calculated from 1.0 pmol injection, at a signal-to-noise ratio of 3, are 10.6-37.8 fmol. The mean interday accuracy ranges from 94 to 105% for fluorescence detection with the largest mean %CV < 7.5. The mean interday precision for all standards is < 6.0% of the expected concentration. Excellent linear responses are observed with coefficients of > 0.9997. |
关键词 | Column Liquid Chromatography Derivatization Amines 1 2-benzo-3 4-dihydrocarbazole-9-isopropyl Chloroformate |
WOS标题词 | Science & Technology ; Life Sciences & Biomedicine ; Physical Sciences |
学科领域 | 生物化学 |
关键词[WOS] | PERFORMANCE LIQUID-CHROMATOGRAPHY ; SOLID-PHASE MICROEXTRACTION ; SECONDARY ALIPHATIC-AMINES ; MASS-SPECTROMETRY ; WASTE-WATER ; 9-FLUORENYLMETHYL CHLOROFORMATE ; REAGENT ; ACIDS ; METHANOL ; CHLORIDE |
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:000237350900007 |
引用统计 | |
文献类型 | 期刊论文 |
条目标识符 | http://210.75.249.4/handle/363003/1333 |
专题 | 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, Peoples R China 2.Qufu Normal Univ, Coll Chem Sci, Shandong 273165, Peoples R China |
推荐引用方式 GB/T 7714 | You, JM,Chen, XM,Zhao, XN,et al. Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS[J]. CHROMATOGRAPHIA,2006,63(7-8):337-343. |
APA | You, JM.,Chen, XM.,Zhao, XN.,Su, YR.,Wang, HL.,...&Sun, J.(2006).Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS.CHROMATOGRAPHIA,63(7-8),337-343. |
MLA | You, JM,et al."Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS".CHROMATOGRAPHIA 63.7-8(2006):337-343. |
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