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液-质联用检测人尿中的苯巯基尿酸

Determination of S-phenylmercapturic acid in human urine by HPLC-MS

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【作者】 叶玉杰陈斯琦宋世震梅勇叶方立

【Author】 YE Yujie,CHEN Siqi,SONG Shizhen,MEI Yong,YE Fangli Departments of Pharmacy,Medical College of Wuhan University of Science and Technology,Wuhan 430065,China

【机构】 武汉科技大学医学院药学系武汉科技大学医学院预防医学系

【摘要】 目的建立人尿中苯巯基尿酸的检测方法,并实际测定职业接苯人群尿中苯巯基尿酸的浓度。方法尿样经酸化水解后,调适宜pH值,液液萃取苯巯基尿酸,经高效液相色谱分离,负离子模式电喷雾离子源质谱检测,选择分子离子峰m/z238,峰面积定量。结果该方法在5~320μg/L范围内线性关系良好,r=0.9994±0.0003,检出限1.2μg/L(S/N=3),回收率在86.8%~94.2%之间,日内与日间精密度相对标准偏差(RSD)均小于7%;用该法对55名职业接苯工人班末尿中苯巯基尿酸进行了检测,并对苯巯基尿酸浓度与空气苯浓度进行回归分析(r=0.8035,P<0.05)。结论该方法快速、灵敏,选择性好,结果准确可靠,可用于职业接苯工人班末尿中的苯巯基尿酸的生物监测,亦可用于环境污染中苯吸收的评价。

【Abstract】 Objective To establish the method to determine S-phenylmercapturic acid(S-PMA) in human urine,and the method was actually applied to determine S-PMA concentrations in the human urine from subjects occupationally exposed to benzene.Methods After the urine samples are hydrolyzed by acidification,and modulated to suitable pH value.S-PMA is obtained by liquid-liquid extraction and separated by HPLC.Use negative ion mode electric spray ion source MS to measure,and select the molecular ion peak m /z 238 and quantitative analysis is performed by peak area.Results This method has good linear in the range of 5 -320μg /L,and r = 0.9994 ± 0.0003,and the detection limit is 1.2μg /L(S /N = 3),recovery percentage is 86.8% -94.2%.Both the intra-and inter-day precisions are less than 7%.Use this method to measure the S-PMA in the end-of-shift urine of 55 workers occupationally exposed to benzene and perform the regression analysis for the S-PMA concentration and the benzene concentration in air(r = 0.8035,P < 0.05).Conclusion The method established by this research is rapid,sensitive and selective,and the results are accurate and reliable.

【基金】 国家科技部基金资助项目子课题(No2006BAK04A11)
  • 【文献出处】 卫生研究 ,Journal of Hygiene Research , 编辑部邮箱 ,2010年05期
  • 【分类号】R96
  • 【被引频次】1
  • 【下载频次】248
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