尿中7种苯系物代谢产物测定的实时肌酐校正法
Simultaneous determination for metabolites of benzene compounds in urine by high performance liquid chromatography
摘要目的:建立一种同时测定尿中7种苯系物代谢产物并实时进行肌酐校正的高效液相色谱法。方法:尿样加入盐酸和过量氯化钠后,加入乙腈∶异丙醇(9∶1)溶液提取待测物,离心后取上清液进样,经反向C18柱分离定性,二极管阵列检测器测定代谢产物和肌酐含量。结果:各代谢产物在2.00 mg/L~100 mg/L的浓度范围内呈良好的线性关系,相关系数均大于0.999,方法检出限为4.15~70.7 μg/L,定量下限为13.8~235 μg/L;测定高、中、低三个添加浓度的加标回收率为85.4%~105.5%,相对标准偏差为1.78%~8.23%( n=6)。 结论:本法经过方法学验证,操作简单,灵敏度高,重现性好,可以满足尿液中7种苯系物代谢产物及肌酐的同时检测。
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abstractsObjective:To describe for the determination of contents of metabolites of benzene compounds in urine sample by high performance liquid chromatography.Methods:After acidification with hydrochloric acid, metabolites in urine were first extracted by acetonitrile and isopropanol (V∶V, 9∶1) with excessive sodium chloride, then gradient separated on a C18 column and then determined by DAD detector.Results:There were good linear relationship between peak areas and injection quality in range of 2.00-100 mg/L ( r>0.999). The detection limit and quantitative limit of this method were 4.15-70.7 μg/L and 13.8-235 μg/L respectively. The precision for the analysis of urine was1.78%-8.23% ( n =6). The average recovery of metabolites was 85.4%-105.5% at thee spiked levels in the range of 2.00-100 mg/L. Conclusion:The accuracy and reproducibility obtained make this method useful for the biological monitoring of occupational exposure to toluene, xylene, styrene and ethylbenzene.
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