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6 mol·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(4.6 mm×200 mm,5 μm)色谱柱分离,于激发波长(λex) 333 nm和发射波长(λem) 390 nm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。

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, 5 μm). 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 6.3×10-15-1.8×10-13mol. 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%.