高效液相色谱-质谱法测定青藏高原植物和土壤样品中氨基酸  

HPLC-MS Determination of Amino Acids in Plants and Soil of Qing-Zang Plateau

作　　者：刘素娟[1] 尤进茂[2,3] 

机构地区：[1]牡丹江师范学院化学化工学院,牡丹江157012 [2]曲阜师范大学化学科学学院,曲阜273165 [3]中国科学院西北高原生物研究所,西宁810001

出　　处：《理化检验（化学分册）》2011年第3期257-260,265,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金项目(20075016);山东省自然科学基金项目(02BS046);牡丹江师范学院科研基金项目资助(QY201005)

摘　　要：提出了高效液相色谱-质谱法测定青藏高原植物和土壤样品中氨基酸的含量。样品中氨基酸经6mol·L^(-1)盐酸溶液提取,加入衍生试剂1,2-苯并-3,4-二氢咔唑-9-乙基氯甲酸酯(BCEOC)进行衍生化反应,衍生化产物经Hypersil BDS C_(18)(4.6mm×200mm,5μm)色谱柱分离,于激发波长(λ_(ex))333 nm和发射波长(λ_(em))390nm进行荧光检测定量,用质谱法定性。色谱分离中采用不同体积比的乙腈与水的混合溶液梯度洗脱,在质谱检测中采用电喷雾离子源正离子模式。方法的检出限(3S/N)为6.3×10^(-15)～1.8×10^(-13)mol之间。以土壤样品为基体,加入20种氨基酸标准作回收试验,测得回收率在89.0%～107.0%之间。HPLC-MS was applied to the determination of amino acids in plants and soil of Qing-Zang plateau. The amino acids were extracted from the sample with 6 mol· L^-1 HCl solution and derivatized with 1,2-benzo-3,4- dihydrocarbazole-9-ethyl chloroformate （BCEOC）. The derivatized products were separated by gradient elution with mixed solution of acetonitrile and water of different ratios on Hypersil BDS C18 column （4. 6 mm× 200 mm, 5μm）. The amino acids were determined by fluorescence detector at the wavelength of 333 nm （λex） and 390 （λem） and identified by MS with ES1＋. Detection limits （3S/N） found were in the range of 6. 3×10^-15～1.8×10^-13mol. Standards of 20 amino acids were added to extracts of soil sample and tested for the recovery; values of recovery obtained were in the range from 89.0% to 107.0%.

关 键 词：高效液相色谱-质谱法 荧光检测 氨基酸 柱前衍生化 青藏高原植物和土壤 

分 类 号：O657.63[理学—分析化学]