反相高效液相色谱法_柱前衍生(期刊论文)

AQC柱前衍生反相高效液相色谱法测定土壤中氨基酸

http://www.100md.com 《分析化学》 2006年第10期

反相高效液相色谱法,柱前衍生,6氨基喹啉基N羟基琥珀酰亚氨基甲酸酯(AQC),氨基酸,土壤,质谱,,反相高效液相色谱法，柱前衍生，6氨基喹啉基N羟基琥珀酰亚氨基甲酸酯(AQC)，氨基

     摘要以2氨基丁酸为内标物，6氨基喹啉基N羟基琥珀酰亚氨基甲酸酯(AQC)为柱前衍生试剂，用XTerra C18 柱，1.8 mmol/L甲酸铵溶液(pH=3.0)和乙腈为流动相，采用梯度洗脱，光电二极管(PDA)检测器在248 nm波长处检测，建立了一种利用反相高效液相色谱同时测定土壤中17种氨基酸的分析方法。方法重现性好，精密度高，氨基酸浓度在25～600 μmol/L范围内，线性相关系数均大于0.99；各氨基酸检出限≤0.5 pmol 。并且在该色谱条件下，获得了灵敏度较高，彼此分离良好的17种AQC衍生氨基酸的LCMS 质谱总离子流图，为今后土壤氨基酸的深入研究提供了更加有利的手段。

    关键词反相高效液相色谱法，柱前衍生，6氨基喹啉基N羟基琥珀酰亚氨基甲酸酯(AQC)，氨基酸，土壤，质谱

    Simultaneous Determination of Amino Acids in Soil by Reversed Phase High Performance Liquid Chromatography by Using 6AminoquinolyNhydroxysuccinimidyl Carbamate

    as a Precolumn Derivatization Reagent

    Hou Songmei, Sun Jing, He Hongbo, Zhang Xudong, Wang Yanhong

    1Key Laboratory of Terrestrial Ecological Process, Institute of Applied Ecology, Chinese Academy of Sciences， Shenyang 110016

    2The Graduate School of Chinese Academy of Sciences, Beijing 10039

    3Department of Chemistry, NorthEast University, Shenyang 110004

    4National Field Observation and Research Station of Shenyang AgroEcosystems, Shenyang 110016

    Abstract A reversedphase high performance liquid chromatographic method for simultaneous determination of 17 amino acids in soil was established. The amino acid samples were mixed with 2aminobutyric acid as the internal standard, derivatized with 6aminoquinolylNhydroxysuccinimidyl carbamate (AQC), and then separated on a XTerra C18 column using 1.8 mmol/L formate ammonium (pH=3.0)and acetonitrile solution as a mobile phase with gradient elution technique. The photodiode detector at 248 nm was utilized for amino acid quantification. All 17 amino acid derivatives were separated well when an optimized elution condition was applied. Consequently, good reproducibility, high sensitivity and high precision of the method were achieved. When the amino acid concentration was set at the range of 25-600 μmol/L, the linear correlation coefficients of the amino acids were above 0.99 and the detector limit of each amino acids was lower than 0.5 pmol. Total ion current chromatograms of mass spectrum of 17 AQC derivatized amino acids were obtained. The method provids a new way for intensifying the study of amino acids in soil and environment. ......

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