论文部分内容阅读
目的研究尿中丁二烯代谢产物1,2-双羟基-4-(N-乙酰半胱氨酸)-丁烷(DHBMA)和1-(N-乙酰半胱氨酸)-2-羟基-3-丁烯(MHBMA)的超高效液相色谱-质谱/质谱(UPLC-ESI-MS/MS)测定方法,对丁二烯暴露工人进行生物监测。方法尿液经1∶10稀释[100μl尿样+50μl混合内标应用液+850μl流动相A(15 mmol/L乙酸铵,p H=6.8)],涡旋混匀,过膜后直接进样,UPLC-ESI-MS/MS测定,工作曲线内标法定量。结果 DHBMA的定量检出限为0.50μg/L,尿中最低检出质量浓度为5.0μg/L,线性相关系数>0.996,高、中、低浓度加标回收率为93%~106%;MHBMA的定量检出限为0.07μg/L,尿中最低检出质量浓度为0.70μg/L,线性相关系数>0.998,高、中、低浓度加标回收率为84%~106%。结论 UPLC-ESI-MS/MS法测定丁二烯代谢产物DHBMA和MHBMA浓度的各项技术指标均能满足生物样品监测的要求,可用于职业场所工作人员的生物监测。
OBJECTIVE To investigate the effects of urinary butadiene metabolites 1,2-dihydroxy-4- (N-acetylcysteine) -butane (DHBMA) and 1- (N-acetylcysteine) 3-Butene (MHBMA) by UPLC-ESI-MS / MS was used to monitor butadiene exposed workers. Methods Urine was diluted 1: 10 [100 μl of urine sample + 50 μl of mixed internal standard solution + 850 μl of mobile phase A (15 mmol / L ammonium acetate, p H = 6.8)] and vortex to mix. , UPLC-ESI-MS / MS determination, working curve internal standard method. Results The detection limit of DHBMA was 0.50μg / L, the lowest detected concentration in urine was 5.0μg / L, the linear correlation coefficient was> 0.996. The recoveries of high, medium and low concentrations were 93% -106%. The recoveries of MHBMA The detection limit was 0.07 μg / L, the lowest detected concentration in urine was 0.70 μg / L, and the linear correlation coefficient was> 0.998. The recoveries were 84% -106% for high, medium and low concentrations. Conclusion The UPLC-ESI-MS / MS method for the determination of butadiene metabolites DHBMA and MHBMA concentrations meet the requirements of biological sample monitoring, which can be used for biological monitoring of occupational staff.