高效液相色谱-串联质谱法测定尿液中丙烯醛的代谢产物
HPLC-MS/MS Determination of the Metabolite of Acrolein in Urine
摘 要
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-15N-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10.0~2 500 mg·L-1,检出限(3S/N)为0.99 μg·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。
丙烯醛
代谢产物
尿液
HPLC-MS/MS
Acrolein
Metabolite
Urine
Abstract
HPLC-MS/MS was applied to the determination of 3-hydroxypropyl mercapturic acid (3-HPMA), the metabolite of acrolein, in human urine.The frozen urine sample was unfrozen at room temperature and centrifugalized. 3-HPMA-15N-13C3 as internal standard was added to the supernatant. 3-HPMA in the supernatant was extracted with acetonitrile. The extract was separated on a Diamonsil C18(2) column, with a mixture of 0.1% (φ) acetic acid solution and methanol as the mobile phase for gradient elution. ESI and SRM were adopted in MS. The linearity range of 3-HPMA was 10.0-2 500 mg·L-1, with detection limit (3S/N) of 0.99 μg·L-1. Recovery rates obtained by standard addition method were in the range of 88.4%-104% and RSDs (n=6) were in the range of 0.7%-2.7%. The method was used to determine 3-HPMA in 15 samples of human urine from smokers and non-smokers. It was found that the average content of 3-HPMA in the urines from smokers were about 7.6 times of that in the urines from non-smokers.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201601003
所属栏目 试验与研究周国俊zhougj@zjtobacco.com
基金项目 2013年度浙江省重大科技专项项目(2013C03050); 浙烟工技(2013)47号项目(ZJZY2013C001)
收稿日期 2015/1/2
修改稿日期
网络出版日期
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备注肖卫强(1984-),男,江西吉安人,工程师,硕士,主 要从事烟草化学的研究工作。
引用该论文: XIAO Wei-qiang,HUANG Jian,YUAN Kai-long,HU An-fu,WU Xi-mei,LIU Jin-li,XIA Qian,DAI Lu,ZHOU Guo-jun. HPLC-MS/MS Determination of the Metabolite of Acrolein in Urine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(1): 11～14
肖卫强,黄健,袁凯龙,胡安福,吴希美,刘金莉,夏倩,戴路,周国俊. 高效液相色谱-串联质谱法测定尿液中丙烯醛的代谢产物[J]. 理化检验－化学分册, 2016, 52(1): 11～14
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【8】李阳,邵敏,陆思华.热解析-GC-MS方法测定大气中的羰基化合物［J］.环境化学, 2009,28(5):630-635.
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