脂肪胺的高效液相色谱分离及质谱鉴定

色谱

脂肪胺的高效液相色谱分离及质谱鉴定

陈向明石运伟赵先恩张海峰尤进茂

College of Chemistry Science, Qufu Normal University, Qufu 273165, China

收稿日期:2004-11-29 修回日期:1900-01-01 出版日期:2005-11-30 发布日期:1987-12-25
通讯作者: 尤进茂

Determination of Aliphatic Amines by High Performance Liquid Chromatography with Fluorescence and Atmospheric Pressure Chemical Ionization Detection and Identification by Mass Spectrometry

CHEN Xiangming, SHI Yunwei, ZHAO Xian’en, ZHANG Haifeng, YOU Jinmao

College of Chemistry Science, Qufu Normal University, Qufu 273165, China

Received:2004-11-29 Revised:1900-01-01 Online:2005-11-30 Published:1987-12-25

摘要/Abstract

摘要：

采用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-乙酸(BCAA)为柱前衍生化试剂,在Hypersil BDS-C18色谱柱上,通过梯度洗脱对12种游离脂肪胺进行了分离和在线质谱定性。以乙腈为溶剂,1-乙基-3-(3-二甲氨基丙基)环己碳二亚胺(EDAC)为缩合剂,在50 ℃条件下衍生反应15 min后获得稳定的荧光产物。激发波长和发射波长分别为333 nm和390 nm。采用大气压化学电离源(APCI)的正离子模式,实现了土壤和污水中脂肪胺的定性及其含量的测定。脂肪胺的线性相关系数大于0.9993,检测限为12~28 fmol。

关键词: 高效液相色谱-质谱, 荧光检测, 脂肪胺 , 柱前衍生

Abstract:

Aliphatic amines exist widely in nature. Therefore, quick and precise determination of aliphatic amines is of great significance. A simple and highly sensitive method based on the derivatization of aliphatic amines utilizing 1,2-benzo-3,4-dihydrocarbazole-9-acetic acid (BCAA) as the novel pre-column derivatization reagent followed by high performance liquid chromatography with fluorescence detection and online mass spectrometric identification was developed. Optimum derivatization was obtained by the reaction of aliphatic amines with BCAA at 50 ℃ for 15 min in the presence of 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDAC) in acetonitrile solvent. The condition of derivatization was mild and the yield of derivative each aliphatic amine was higher than 94%. Derivatives were sufficiently stable to be efficiently analyzed by high performance chromatography without pretreatment. On a reversed-phase BDS-C18 column, twelve aliphatic amine derivatives (C1-C12) were separated under gradient elution with baseline resolution. The precise determining aliphatic amines from soil and wastewater samples was obtained by post-column online mass spectrometric identification with atmospheric pressure chemical ionization(APIC) source under positive mode detection. The established method exhibited excellent reproducibility and recovery. Linear responses were observed with coefficients over 0.9993. The detection limits (at signal-to-noise ratio of 3∶1) were 12-28 fmol.

Key words: aliphatic amines , fluorescence detection, pre-column derivatization, high performance liquid chromatography-mass spectrometry

陈向明石运伟赵先恩张海峰尤进茂.

脂肪胺的高效液相色谱分离及质谱鉴定

[J]. 色谱.

CHEN Xiangming, SHI Yunwei, ZHAO Xian’en, ZHANG Haifeng, YOU Jinmao.

Determination of Aliphatic Amines by High Performance Liquid Chromatography with Fluorescence and Atmospheric Pressure Chemical Ionization Detection and Identification by Mass Spectrometry

[J]. Chinese Journal of Chromatography.

HTML			PDF

最新录用	在线预览	正式出版	最新录用	在线预览	正式出版
0	0	0	0	0	28

来源	本网站	其他网站

次数	27	1
比例	96%	4%

摘要

最新录用	在线预览	正式出版

0	0	39

	来源	本网站

	次数	39
	比例	100%

[1]	张莹, 杨静, 马跃新, 曹玲, 黄青. 基于超高效液相色谱-质谱法的肽段分析中非特异性吸附评估及通用型最小化策略[J]. 色谱, 2022, 40(7): 616-624.
[2]	刘婷婷, 王琪, 叶翰章, 孔佳, 李宇浩, 顾婧婧, 丁永立, 张占恩, 王学东. 磁性三维氮掺杂碳纳米材料对6种双酚类化合物的吸附性能及其在泡腾分散微萃取中的应用[J]. 色谱, 2022, 40(12): 1049-1063.
[3]	曲栗, 古淑青, 张嘉麒, 赵超敏, 邓晓军. 柱前衍生-超高效液相色谱法测定3种奶粉中18种氨基酸[J]. 色谱, 2021, 39(5): 472-477.
[4]	李慧, 崔兰冲, 章国磊, 张萌萌, 焦丽丽, 吴巍. 超高效液相色谱-串联质谱法定量分析尿液中色氨酸及其代谢产物[J]. 色谱, 2021, 39(5): 518-525.
[5]	牟红梅, 慈志娟, 艾沙江·买买提, 梁艳萍, 刘笑宏, 杜晓云, 于强, 李庆余, 李元军. 基于非靶向代谢组学的茄梨和红茄梨成熟期果皮代谢产物的差异分析[J]. 色谱, 2021, 39(11): 1203-1212.
[6]	白洁, 王妲, 刘泽平, 张佳琪, 刘丽艳, 韩艳梅. 柱前衍生-高效液相色谱法同时测定血清中氨基酸类及单胺类神经递质[J]. 色谱, 2020, 38(8): 923-928.
[7]	王荣, 周敏, 王苏霞, 廖原, 樊雪, 马永钧. 柱前衍生毛细管电泳-电致化学发光法测定日用化妆品中的氨甲环酸含量[J]. 色谱, 2020, 38(8): 968-974.
[8]	孙珊珊, 公丕学, 张艳侠, 王明栋, 卢兰香, 李新玲, 薛霞, 刘艳明, 张峰. 柱后还原-高效液相色谱法同时测定调制乳粉中维生素K₁和维生素K₂[J]. 色谱, 2020, 38(7): 847-852.
[9]	徐坤, 金钰龙, 黄嫣嫣, 赵睿. 超高效液相色谱-质谱联用法监测人心房钠尿肽的化学合成[J]. 色谱, 2020, 38(3): 324-331.
[10]	赵兴云, 张红燕, 周孝禹, 王莉, 万丽红, 吴仁安. 核壳硅碳复合微球固定相的制备及其在糖类分离中的应用[J]. 色谱, 2020, 38(12): 1357-1362.
[11]	赵孟欣, 王泽岚, 孟哲, 李吉光, 李和平, 刘万毅. 温和条件下柱前标记-高效液相色谱-质谱法测定枸杞多糖中单糖组成[J]. 色谱, 2019, 37(11): 1162-1172.
[12]	韩疏影, 宋易霖, 康安, 邓海山, 朱栋, 池玉梅. 在线富集与高效液相色谱-荧光检测法联用同时检测儿童水杯中9种双酚类物质[J]. 色谱, 2019, 37(11): 1185-1192.
[13]	叶美君, 陆小磊, 刘相真, 张海华, 杜颖颖, 潘胜东. 柱前衍生-超高效液相色谱-串联质谱测定茶叶中草甘膦、草铵膦及主要代谢物氨甲基膦酸残留[J]. 色谱, 2018, 36(9): 873-879.
[14]	汤娟, 周佳, 钱凯, 丁友超, 程月, 齐琰. 超高效液相色谱法同时测定纺织品中18种荧光增白剂[J]. 色谱, 2018, 36(7): 670-677.
[15]	肖汉, Kevin YAN, 郑怡婷, 王彦, 阎超. 基于加压毛细管电色谱-激光诱导荧光联用技术研究离子强度对维生素B₂光解反应的影响[J]. 色谱, 2018, 36(4): 381-387.