Sakura N, Nishimura S, Fujita N, Namera A, Yashiki M, Kojima T
Hiroshima University School of Medicine, Japan.
J Chromatogr B Biomed Sci Appl. 1998 Nov 20;719(1-2):209-12. doi: 10.1016/s0378-4347(98)00422-8.
A rapid and sensitive headspace gas chromatographic and mass spectrometric (GC-MS) method was developed for the determination of acrolein in human urine. A 0.5-ml urine sample in a glass vial containing propionaldehyde as an internal standard was heated at 80 degrees C for 5 min. A 0.1-ml volume of headspace vapor was injected into a GC-MS instrument. Acrolein and propionaldehyde were coeluted at 3.1 min using a DB-1 capillary column, and well separated by selective ion monitoring (SIM) mode using ions m/z 56.05 and m/z 58.05. The interassay and intraassay coefficient of variation were 0.99% and 3.3%. The calibration curve demonstrated a good linearity throughout concentrations ranging from 1 to 1000 nM. However, due to a wide variation of acrolein evaporation rates from human urine, a calibration curve must be established for each urine specimen using a standard addition method and detection limit varied from 1 to 5 nM. The total analysis time for two samples from one urine specimen required about 15 min. Therefore, this method is convenient for the urgent monitoring of urinary acrolein in patients to whom alkylating agents are administered.
建立了一种快速灵敏的顶空气相色谱-质谱联用（GC-MS）法测定人尿中丙烯醛。将0.5 ml尿样置于含有丙醛作为内标的玻璃小瓶中，在80℃加热5分钟。取0.1 ml顶空气体注入GC-MS仪器。使用DB-1毛细管柱时，丙烯醛和丙醛在3.1分钟共洗脱，通过选择离子监测（SIM）模式，使用m/z 56.05和m/z 58.05离子可实现良好分离。批间和批内变异系数分别为0.99%和3.3%。校准曲线在1至1000 nM的浓度范围内呈现良好线性。然而，由于人尿中丙烯醛蒸发速率差异很大，必须使用标准加入法为每个尿样建立校准曲线，检测限在1至5 nM之间变化。对一个尿样的两个样品进行分析的总时间约为15分钟。因此，该方法便于对接受烷化剂治疗的患者进行尿中丙烯醛的紧急监测。
