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文摘
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利用新型荧光试剂2-(2-(10-蒽基)-苯并咪唑)-乙酸(ABIA)为柱前衍生化试剂,在Akasil-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, N-乙基-N′-[(3-二甲氨基)丙基]碳二亚胺盐酸盐(EDC)为缩合剂,在50℃条件下衍生反应20 min后获得稳定的荧光产物. 激发波长和发射波长分别为260 nm和430 nm,采用大气压化学电离源(APCI)的正离子模式,实现了土壤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0.9990,检出限为11.72 ~25.63 fmol. |
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其他语种文摘
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A simple and highly sensitive method based on the derivatization of aliphatic amines with 2-(2-(anthracen-9-yl)-1H-benzo[d]imidazoL~(-1)-yl)acetic acid(ABIA) as the novel pre-column derivatization reagent followed by high performance liquid chromatography with fluorescence detection and on line mass spectrometric identification was developed. Derivatization was obtained by the reaction of aliphaticamines with ABIA at 50℃for 20 min in the presence of N-ethyl-N′-(3-dimethylamino propyl) carbodiimide hydrochloride (EDC) in acetonitrile solvent. Derivatives were sufficiently stable to be efficiently analyzed by high performance chromatography without pretreatment. On a reversed phase Akasil-C18 column, twelve aliphaticamine derivatives(C_1~C_(12)) were separated under gradient elution with an excitation maximum atλ_(ex)260 nm and an emission maximum atλ_(em)430 nm. The precise determining aliphatic amines in soil samples was obtained by post-column on line mass spectrometric identification with atmospheric pressure chemical ionization (APCI) source under positive mode detection. The established method exhibited excellent reproducibility and recovery. Linear responses were observed with coefficients over 0.9990. The detection limits (at signal-to-noise ratio of 3:1) were 11.72~25.63 fmol. |
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来源
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分析科学学报
,2010,26(3):261-265 【核心库】
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关键词
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液相色谱-质谱
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荧光检测
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柱前衍生
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脂肪胺
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地址
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1.
曲阜师范大学化学与化工学院, 山东省生命有机分析重点实验室, 山东, 曲阜, 273165
2.
中国科学院西北高原生物研究所, 青海, 西宁, 810001
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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1006-6144 |
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学科
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化学 |
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基金
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国家自然科学基金
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中国科学院“百人计划”项目
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文献收藏号
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CSCD:3926185
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