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目的采用超高效液相色谱串联质谱法测定人血清中5-羟基吲哚乙酸(5-HIAA)的含量。方法采用Waters Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm),流动相为2.5 mmol·L-1乙酸铵水溶液(含0.02%甲酸)-甲醇(68∶32),流速0.2 m L·min-1,进样量3μL,柱温35℃,样品室温度6℃;采用电喷雾正离子模式电离,5-HIAA和甲氨蝶呤内标的监测离子分别为m/z 192.2→146.0、m/z 455.3→308.2。结果 5-HIAA的线性范围为0.0100~10.02μmol·L-1,平均回收率为92.1%~96.5%,批内、批间RSD均小于15%。结论所用方法的线性范围宽、分析时间短,可用于神经内分泌肿瘤的诊断及进展监测。
Objective To determine the content of 5-hydroxyindoleacetic acid (5-HIAA) in human serum by ultra performance liquid chromatography-tandem mass spectrometry. Methods Waters Acquity UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm) was used. The mobile phase consisted of 2.5 mmol·L -1 ammonium acetate aqueous solution (containing 0.02% formic acid) -methanol (68:32) Min-1, the injection volume 3μL, column temperature 35 ℃, sample room temperature 6 ℃; using electrospray positive ion mode ionization, 5-HIAA and methotrexate internal standard monitoring ions were m / z 192.2 → 146.0, m / z 455.3 → 308.2. Results The linear range of 5-HIAA was 0.0100 ~ 10.02μmol·L-1, the average recovery was 92.1% -96.5%. The intra-assay and inter-assay RSD were less than 15%. Conclusions The method used has a wide linear range and short analysis time. It can be used for the diagnosis and progression monitoring of neuroendocrine tumors.