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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
【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%.
【Key words】 HPLC-MS; Fluorescence detection; Amino acids; Pre-column derivatization; Plants and soil of Qing-Zang plateau;
- 【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