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[目的]通过高效液相色谱(HPLC)与液质联用(LC/MS)检测尿中苯巯基尿酸(SPMA)的方法比对,评价HPLC方法的可行性。[方法]尿样经50%硫酸酸化、氯仿:异丙醇(体积比为5:1)萃取,挥干残渣用甲醇溶解后经十八烷基硅烷(ODS)柱分离,分别采用紫外检测器和质谱检测器检测;对86名职业苯接触者尿样采用两种方法比对分析,以LC/MS分析数据评定HPLC测定结果的有效性。[结果]HPLC方法和LC/MS方法对SPMA的检出限(LOD)分别为40μg/L和10μg/L,SPMA保留时间分别为31 min和7.8 min左右。86份尿样中有13份为假阳性,两方法检测结果的相关系数为0.915,但HPLC检测数据高估LC/MS数据8%~21%。[结论]HPLC法可作为职业苯接触者生物监测的初步筛检方法,LC/MS可准确定量测定尿中SPMA浓度。
[Objective] To evaluate the feasibility of HPLC method for the comparison of urinary phenylmercapturic acid (SPMA) with high performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC / MS). [Method] The urine sample was acidified with 50% sulfuric acid and extracted with chloroform and isopropanol (5: 1 by volume). The residue was dissolved in methanol and separated by octadecylsilane (ODS) column. And mass spectrometry detector. The urine samples from 86 occupational benzene exposures were analyzed by two methods and the data of HPLC were evaluated by LC / MS. [Result] The detection limits (LODs) of SPMA by HPLC and LC / MS were 40μg / L and 10μg / L, respectively. The retention time of SPMA was 31 min and 7.8 min, respectively. Of the 86 urine samples, 13 were false positives. The correlation coefficient between the two methods was 0.915, but the HPLC data overestimated the LC / MS data by 8% -21%. [Conclusion] HPLC method can be used as a preliminary screening method for biological monitoring of occupational benzene exposures. LC / MS can accurately determine the concentration of SPMA in urine.