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.
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 Ciscolumn 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 When the amino acid concentration was set at the range of 25 and high precision of the method were achieved. -- 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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第10期1395-1400,共6页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.40471068)
中国科学院知识创新工程重要方向项目(No.kzcx3-sw-433)资助
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
氨基酸
土壤
质谱
Reversed phase high performance liquid chromatography, pre-column derivatizatiion, 6-aminoquinoly-N-hydroxysuccinimidyl carbamate, amino acids, soil, mass spectrometric
