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采用高效液相色谱-串联质谱法测定人体尿液中丙烯醛的代谢产物N-乙酰基-S-(3-羟基丙基)半胱氨酸(3-HPMA)。冰冻的人体尿液在室温下解冻、离心后,在上清液中加入3-HPMA-15 N-13C3作内标,用乙腈萃取其中的3-HPMA。萃取液经Diamonsil C18(2)色谱柱分离,以0.1%(φ)乙酸-甲醇混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾电离源和选择反应监测模式。3-HPMA的线性范围为10.0~2 500mg·L-1,检出限(3S/N)为0.99μg·L-1。加标回收率在88.4%~104%之间,测定值的相对标准偏差(n=6)在0.7%~2.7%之间。采用该方法测定了15例尿液样本,吸烟者尿液中3-HPMA的平均含量为非吸烟者的7.6倍。
The metabolite of acrolein, N-acetyl-S- (3-hydroxypropyl) cysteine (3-HPMA) in human urine was determined by high performance liquid chromatography-tandem mass spectrometry. Frozen human urine is thawed at room temperature. After centrifugation, 3-HPMA-15 N-13C3 is added as an internal standard to the supernatant and the 3-HPMA is extracted with acetonitrile. The extract was separated on a Diamonsil C18 (2) column and eluted with a gradient of 0.1% (?) Acetic acid-methanol. Electrospray ionization and selective reaction monitoring are used in mass spectrometry. The linear range of 3-HPMA was 10.0-2,500 mg · L -1, and the detection limit (3S / N) was 0.99 μg · L -1. The spiked recoveries ranged from 88.4% to 104%, and the relative standard deviations (n = 6) of the measured values ranged from 0.7% to 2.7%. Using this method, 15 urine samples were determined. The mean urinary 3-HPMA content of smokers was 7.6 times higher than that of non-smokers.