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目的推荐我国职业接触苯尿中反-反式黏糠酸(ttMA)生物限值并建立相应的高效液相色谱(HPLC)测定方法。方法选择职业苯接触者56人和非苯接触者24人,应用活性炭吸附管采集工人呼吸带空气、CS2洗脱、毛细管气相色谱法检测个体外暴露水平,同时采集当日工作班前和班末尿样本,应用HPLC测定尿中ttMA以观察内暴露水平。尿样经2 mol／L盐酸酸化、香草酸为内标、乙酸乙酯萃取预处理,采用ODS柱、冰乙酸:四氢呋喃:甲醇:水(体积比1:2:10:87)为流动相、流速0．9 ml／min、紫外检验波长264 nm、柱温25℃的色谱条件分离测定尿中ttMA。结果ttMA的线性范围为0．10-10．00 mg/L．检出限为0．10 mg/L,加标平均回收率为95．1％-100．5％,批内、批间精密度变异系数分别为4．4％-7．5％和6．2％-8．8％。接苯工人空气苯浓度范围0．332-146．000 mg/m3,平均浓度41．8 mg／m3,班末尿ttMA与个体苯接触量存在良好线性关系y(mg/g Cr)=2．103+0．177x(mg/m3),r=0．791,P<0．01,将我国职业苯接触限值PC-TW A=6 mg/m3代入回归方程,推算工作班末尿中ttMA含量为3．165 mg／g Cr。结论建立的HPLC测定ttMA方法简便、快速、灵敏,可用于职业接触苯的生物监测,参考国内外文献和国外相关标准,建议我国职业接触苯生物限值班末尿ttMA为2．4 mmol／mol Cr(3．0 mg／g Cr)。
Objective To recommend the bioassay limit of ttMA in benzeneuria of our country and to establish the corresponding high performance liquid chromatography (HPLC) method. Methods Sixty-six benzene-exposed workers and 24 non-benzene-exposed workers were enrolled in this study. Air from the respiratory zone of workers was collected by activated charcoal absorption tube. The exposure to CS2 was detected by capillary gas chromatography. Meanwhile, Samples, urine ttMA HPLC determination of the level of exposure. The urine sample was acidified with 2 mol / L hydrochloric acid, vanillic acid was used as internal standard and pretreated with ethyl acetate. The mobile phase consisted of ODS column and tetrahydrofuran: methanol: water (1: 2: 10: 87) Flow rate 0.9 ml / min, UV detection wavelength 264 nm, column temperature 25 ℃ chromatographic separation and determination of urinary ttMA. Results The linear range of ttMA was 0.10-10.00 mg / L. The detection limit was 0.10 mg / L, and the average recoveries were 95.1% -100.5%. The coefficients of variation of intra-and inter-batch precision were 4.4% -7.5% and 6 respectively. 2% -8.8%. The benzene concentration in the benzene-exposed workers ranged from 0.332 to 146.000 mg / m3 with an average concentration of 41.8 mg / m3. There was a good linear relationship between the ttMA of urine and the benzene exposure of the individual y (mg / g Cr) = 2. 103 + 0.177x (mg / m3), r = 0.791, P <0.01, the occupational benzene exposure limit PC-TW A = 6 mg / m3 was substituted into the regression equation, The content is 3.165 mg / g Cr. Conclusion The established method for the determination of ttMA by HPLC is simple, rapid and sensitive and can be used for biological monitoring of occupational exposure to benzene. Reference to domestic and foreign literatures and relevant foreign standards, it is suggested that the ttMA of benzene in the end-use benzene of occupational exposure to benzene in our country is 2.4 mmol / mol Cr (3.0 mg / g Cr).