Ye Yujie, Chen Siqi, Song Shizhen, Mei Yong, Ye Fangli
Department of Pharmacy, Medical College of Wuhan University of Science and Technology, Wuhan 430065, China.
Wei Sheng Yan Jiu. 2010 Sep;39(5):536-9.
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.
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.
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).
The method established by this research is rapid, sensitive and selective, and the results are accurate and reliable.
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。
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。
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)。
本研究建立的方法快速、灵敏、选择性好,结果准确可靠。