色谱2011，Vol.29Issue(1)：31-35,5.DOI:10.3724/SP.J.1123.2011.00031
固相萃取-高效液相色谱-串联质谱法同时测定尿液中的4种巯基尿酸
Simultaneous determination of four mercapturic acids in human urine using solid phase extraction and liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method was developed for the simultaneous extraction and determination of four mercapturic acids ( MAs), N-acetyl-S- ( 3,4-dihydroxybutyl) -L-cysteine ( DHBMA ), N-acetyl-S( 3-hydroxypropyl ) -L-cysteine ( 3-HPMA ), N-acetyl-S-( 2-carboxyethyl ) -L-cysteine ( CEMA ) and S-phenylmercapturic acid (SPMA), in human urine using solid phase extraction and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Frozen urine samples were thawed at room temperature, and centrifuged to remove any settled precipitate.The supernatant was then purified and concentrated by a C18 solid phase extraction column,and analyzed by HPLC-MS/MS in the multiple reaction monitoring (MRM) mode for the quantitative analysis. The ranges of recovery for DHBMA, 3-HPMA, CEMA and SPMA spiked in human urine matrix at three concentration levels were 105.6％ - 124. 4％, 102.7％ - 106.5％,103.2％ - 103.9％ and 101.7％ - 104.3％, respectively, with the relative standard deviations of 2.6％-7.7％. The limits of detection (LOD, S/N≥3) were 0.062, 0.031, 0.020 and 0.003 μg/L for DHBMA, 3-HPMA, CEMA and SPMA, respectively. The method was successfully used to detect 4 MAs in 37 human urine samples from smokers and non-smokers. It was found that the contents of 3-HPMA, CEMA and SPMA in the urines from cigarette smokers were about three to six-fold more than those in the urines from the non-smokers.关键词
液相色谱-串联质谱/固相萃取/巯基尿酸/尿液分类
化学化工引用本文复制引用
侯宏卫,熊巍,郜娜,宋东奎,唐纲岭,胡清源..固相萃取-高效液相色谱-串联质谱法同时测定尿液中的4种巯基尿酸[J].色谱,2011,29(1):31-35,5.基金项目
云南中烟工业公司科技项目(No. 2010JC11). （No. 2010JC11）
