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[高效液相色谱-质谱法测定人尿液中S-苯巯基尿酸]

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

作者信息

Ye Yujie, Chen Siqi, Song Shizhen, Mei Yong, Ye Fangli

机构信息

Department of Pharmacy, Medical College of Wuhan University of Science and Technology, Wuhan 430065, China.

出版信息

Wei Sheng Yan Jiu. 2010 Sep;39(5):536-9.

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 5-320 microg/L, and r = 0.9994 +/- 0.0003, and the detection limit is 1.2 microg/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.

摘要

目的

建立人尿中S-苯巯基尿酸(S-PMA)的测定方法,并将该方法实际应用于测定职业性接触苯人群的人尿中S-PMA浓度。

方法

尿样经酸化水解后,调节至适宜pH值。通过液-液萃取获得S-PMA,并用高效液相色谱法分离。采用负离子模式电喷雾离子源质谱进行测定,选择分子离子峰m/z 238,以峰面积进行定量分析。

结果

该方法在5 - 320μg/L范围内线性良好,r = 0.9994±0.0003,检测限为1.2μg/L(信噪比=3),回收率为86.8% - 94.2%。日内和日间精密度均小于7%。用该方法测定55名职业性接触苯工人下班时尿样中的S-PMA,并对S-PMA浓度与空气中苯浓度进行回归分析(r = 0.8035,P < 0.05)。

结论

本研究建立的方法快速、灵敏、选择性好,结果准确可靠。

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