Kellert Marco, Scholz Karoline, Wagner Silvia, Dekant Wolfgang, Völkel Wolfgang
Department of Toxicology, University of Würzburg, Versbacher Strasse 9, 97078 Würzburg, Germany.
J Chromatogr A. 2006 Oct 27;1131(1-2):58-66. doi: 10.1016/j.chroma.2006.07.026. Epub 2006 Aug 1.
A sensitive and specific electrospray tandem mass spectrometry method using a column switching unit with two trap columns was established to quantify the mercapturates (MAs) of acrylamide (AA) and glycidamide (GA) in human urine. A specially endcapped material was applied for trapping the hydrophilic MAs and a pre-trap column was used to remove lipophilic compounds from the directly injected urine to protect the trap column. The limits of quantitation for AA-MA and GA-MA in urine were 0.5 microg/L and 1 microg/L, respectively. Urine was spiked with deuterated internal standards and injected directly into LC-MS/MS. Urine of smokers (n=13) revealed the highest concentrations of AA-MA and GA-MA in the range of 61-706 microg/L and 5-54 microg/L, respectively. Lower levels for AA-MA (14-102 microg/L) and GA-MA (1-11 microg/L) were detected in non-smokers (n=13).
建立了一种灵敏且特异的电喷雾串联质谱法,该方法使用带有两个捕集柱的柱切换单元,用于定量人尿液中丙烯酰胺(AA)和缩水甘油酰胺(GA)的巯基尿酸盐(MAs)。采用一种特殊的封端材料来捕集亲水性MAs,并使用预捕集柱从直接进样的尿液中去除亲脂性化合物,以保护捕集柱。尿液中AA-MA和GA-MA的定量限分别为0.5μg/L和1μg/L。尿液加入氘代内标后直接进样到液相色谱-串联质谱仪中。吸烟者(n = 13)的尿液中AA-MA和GA-MA的浓度最高,分别在61 - 706μg/L和5 - 54μg/L范围内。在非吸烟者(n = 13)中检测到较低水平的AA-MA(14 - 102μg/L)和GA-MA(1 - 11μg/L)。