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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

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【作者】 刘素娟尤进茂

【Author】 LIU Su-juan~1,YOU Jin-mao~(2,3) (1.Dept.of Chem.and Chem.Eng.,Mudanjiang Normal College,Mudanjiang 157011,China; 2.College of Chemistry,Qufu Normal University,Qufu 273165,China; 3.Northwest Research Institute of Plateau Biology,Chinese Academy of Sciences,Xi’ning 810001,China)

【机构】 牡丹江师范学院化学化工学院曲阜师范大学化学科学学院中国科学院西北高原生物研究所

【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 C18(4.6mm×200mm,5μm)色谱柱分离,于激发波长(λex)333 nm和发射波长(λem)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6.3×10-15~1.8×10-13mol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。

【Abstract】 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 HDS 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 ESI+.Detection limits(3S/N) found were in the range of 6.3×10-15 - 1.8×10-13 mol. 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%.

【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)
  • 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2011年03期
  • 【分类号】Q946;S153.6
  • 【被引频次】6
  • 【下载频次】446
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