Pre-column derivatization of amines with 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate followed by LC-fluorescence and LC-APCI-MS

	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
刊名	chromatographia
	2006-04-01
卷号	63 期号:7-8 页码:337-343
关键词	column liquid chromatography derivatization amines 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl chloroformate
合作状况	其它
中文摘要	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.
英文摘要	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.
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 ; secondary aliphatic-amines ; mass-spectrometry ; waste-water ; 9-fluorenylmethyl chloroformate ; reagent ; acids ; methanol ; chloride
收录类别	SCI
语种	英语
WOS记录号	WOS:000237350900007
公开日期	2009-12-08
内容类型	期刊论文
源URL	[http://ir.nwipb.ac.cn/handle/363003/1333]
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, 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.