Rapid Determination of 4 Mercapturic Acids in Human Urine by UHPLC-MS/MS
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摘 要
1.00 mL人体尿液样品经自制的萃取装置萃取后,收集萃取液,采用超高效液相色谱-串联质谱法快速测定萃取液中4种巯基尿酸的含量。以Waters Acquity UPLCTM BEH C18色谱柱为固定相,以不同体积比的0.05%(体积分数)乙酸溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾负离子源和多反应监测模式,采用内标法定量。4种巯基尿酸的检出限(3S/N)为0.012~0.082 μg·L-1,测定下限(10S/N)为0.038~0.270 μg·L-1。方法用于人体尿液样品的分析,日内回收率为93.9%~102%,日内相对标准偏差(n=7)为2.0%~3.4%,日间回收率为93.4%~102%,日间相对标准偏差(n=7)为2.4%~4.1%。
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Abstract
The sample of human urine (1.00 mL) was extracted by self-made extraction device. The extract was collected. UHPLC-MS/MS was applied to the rapid determination of 4 mercapturic acids in the extract. Waters Acquity UPLCTM BEH C18 chromatographic column was used as stationary phase, and the mixture of 0.05% (φ) acetic acid solution and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Internal standard method was used for quantitative. Detection limits (3S/N) and lower limits of determination (10S/N) of the 4 mercapturic acids were in the ranges of 0.012-0.082 μg·L-1 and 0.038-0.270 μg·L-1 respectively. The proposed method was applied to the analysis of the sample of human urine. Values of recovery and RSDs (n=7) of intra-day were in the ranges of 93.9%-102% and 2.0%-3.4% respectively. Values of recovery and RSDs (n=7) of inter-day were in the ranges of 93.4%-102% and 2.4%-4.1% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201905022
所属栏目 专题报道(高效液相色谱法)
基金项目 云南中烟科技项目(20186JC09)
收稿日期 2018/6/19
修改稿日期
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备注刘欣,博士,主要从事烟草化学分析工作
引用该论文: LIU Xin,KONG Weisong,YANG Yekun,ZHAO Hui,WANG Jin,XU Yong,HUANG Haitao,LI Xuemei,YANG Guangyu,ZHANG Chengming,LI Jing. Rapid Determination of 4 Mercapturic Acids in Human Urine by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(5): 607~611
刘欣,孔维松,杨叶昆,赵辉,王晋,许永,黄海涛,李雪梅,杨光宇,张承明,李晶. 超高效液相色谱-串联质谱法快速测定人体尿液中4种巯基尿酸[J]. 理化检验-化学分册, 2019, 55(5): 607~611
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【9】MAESTRI L, GHITTORI S, IMBRIANI M, et al. A simple high-performance liquid chromatographic method for the determination of urinary N-acetyl-S-(N-methylcarbamoyl)-cysteine (AMCC), the mercapturic acid of N,N-Dimethylformamide (DMF)[J]. Toxicology Letters, 1998,95:197-198.
【2】BAAN R, GROSSE Y, STRAIF K, et al. A review of human carcinogens-Part F:Chemical agents and related occupations[J]. The Lancet Oncology, 2009,10(12):1143-1144.
【3】FENG S, ROETHIG H J, LIANG Q, et al. Evaluation of urinary 1-hydroxypyrene, S-phenylmercapturic acid, trans, trans-muconic acid, 3-methyladenine, 3-ethyladenine, 8-hydroxy-2'-deoxyguanosine and thioethers as biomarkers of exposure to cigarette smoke[J]. Biomarkers, 2006,11(1):28-52.
【4】周元陵,金复生,金泰.生物标志物巯基尿酸的研究进展[J].劳动医学, 2001,18(3):182-183.
【5】侯宏卫,熊巍,郜娜,等.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.
【6】杨雪,谢剑平,谢复炜,等.尿液中1,3-丁二烯代谢产物的液相色谱-串联质谱法检测[J].分析测试学报, 2009,28(6):649-654.
【7】王磊君,李钢,郑赛晶,等.高效液相色谱-质谱联用技术同时测定人体尿液中11种代谢物[J].分析化学, 2015,43(1):121-126.
【8】叶海朋,施燕鹏,邵吉,等.分散液-液微萃取-高效液相色谱法测定尿中苯巯基尿酸[J].中国卫生检验杂志, 2018,28(6):646-649.
【9】MAESTRI L, GHITTORI S, IMBRIANI M, et al. A simple high-performance liquid chromatographic method for the determination of urinary N-acetyl-S-(N-methylcarbamoyl)-cysteine (AMCC), the mercapturic acid of N,N-Dimethylformamide (DMF)[J]. Toxicology Letters, 1998,95:197-198.
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