School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, China.
J Mass Spectrom. 2012 Oct;47(10):1341-6. doi: 10.1002/jms.3084.
A high-performance liquid chromatography coupled with Q-time of flight mass spectrometry (HPLC/Q-TOF MS) method was developed and validated for the determination of 1, 3-diaminopropane, putrescine, cadaverine, spermidine and spermine in human plasma. The plasma samples were first pretreated by 10% HClO(4) and then derived by benzoyl chloride with 1, 6-diaminohexane as internal standard. The derived polyamines were separated on a C(18) column using a gradient program. The detection was performed on a Q-TOF MS by positive ionization mode. Calibration curve for each polyamine was obtained in the concentration range of 0.4 ~ 200.0 ng • ml(-1), with limit of detection of 0.02 ~ 0.1 ng • ml(-1). The intra- and inter-day RSD for all polyamines were 2.5-14.0% and 2.9 ~ 13.4%, respectively. The method was applied to determine the polyamines in human plasma from cancer patients and healthy volunteers. Results showed that the mean levels of polyamines in the plasma of cancer patients were higher than that of healthy volunteers, which suggested that the plasma polyamines could be employed as cancer diagnostic indicators in clinical testing.
建立并验证了一种高效液相色谱-四极杆飞行时间质谱（HPLC/Q-TOF MS）法，用于测定人血浆中的 1,3-二氨基丙烷、腐胺、尸胺、亚精胺和精胺。血浆样品先用 10%高氯酸（HClO(4)）预处理，然后用苯甲酰氯衍生，以 1,6-二氨基己烷为内标。衍生后的多胺在 C(18)柱上采用梯度程序分离。正离子模式下在 Q-TOF MS 上进行检测。各多胺的校准曲线浓度范围为 0.4200.0ng•ml(-1)，检测限为 0.020.1ng•ml(-1)。所有多胺的日内和日间 RSD 分别为 2.514.0%和 2.913.4%。该方法用于测定癌症患者和健康志愿者的人血浆中的多胺。结果表明，癌症患者血浆中多胺的平均水平高于健康志愿者，这表明血浆多胺可作为临床检测中的癌症诊断标志物。
